[ CAS No. 2761-09-3 ] {[proInfo.proName]}

Name: 2761-09-3|3-Hydroxypropyl methacrylate|95% (isomers mixture)(stabilized with MEHQ)
Brand: Ambeed
SKU: A1148347
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Quality Control of [ 2761-09-3 ]

COA NMR CNMR HPLC LC-MS

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Product Details of [ 2761-09-3 ]

CAS No. :	2761-09-3	MDL No. :	MFCD00081136
Formula :	C₇H₁₂O₃	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	-
M.W :	144.17	Pubchem ID :	-
Synonyms :

Safety of [ 2761-09-3 ]

Signal Word:	Warning	Class:	N/A
Precautionary Statements:	P261-P264-P270-P271-P280-P301+P312+P330-P302+P352+P312+P362+P364-P304+P340+P312-P305+P351+P338+P337+P313-P501	UN#:	N/A
Hazard Statements:	H302+H312+H332-H315-H319	Packing Group:	N/A
GHS Pictogram:

Application In Synthesis of [ 2761-09-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

Downstream synthetic route of [ 2761-09-3 ]

[ 2761-09-3 ] Synthesis Path-Downstream 1~28

1
[ 79-41-4 ]
[ 504-63-2 ]
[ 2761-09-3 ]

Yield	Reaction Conditions	Operation in experiment
44%	With 2,6-di-tert-butyl-4-methyl-phenol; toluene-4-sulfonic acid at 85℃; for 5h;	8.6g of methacrylic acid (0.1 mol), 1,3-propanediol 15.2 g (0.2 mol), p-toluenesulfonic acid 0.86 g (0.005 mol), and the BHT0.1g as a polymerization inhibitor Place in a glass container and heat to 85 ° C and stir. The reaction system in the heating and stirring state was brought into a reduced pressure state, and stirring was continued for 5 hours while removing moisture from the reaction system. Thereafter, cooling the resulting liquid, purified by silica gel column chromatography to obtain after concentration, 3-hydroxypropyl methacrylate 6.3 g (44% yield).
44%	With C₂₆H₂₆O₉; toluene-4-sulfonic acid at 85℃; for 5h;	8.6 g (0.1 mol) of methacrylic acid, 15.2 g (0.2 mol) of 1,3-propanediol,0.86 g (0.005 mol) of p-toluenesulfonic acid,and,0.1 g of BHT as a polymerization inhibitor was placed in a glass container,Heated to 85 ° C,Stir.The reaction system in this heating and stirring state is brought into a reduced pressure state,Stirring was continued for 5 hours while removing moisture from the reaction system.after that,The resulting liquid was cooled,After purification and concentration using silica gel column chromatography, 6.3 g (yield 44%) of 3-hydroxypropyl methacrylate was obtained.
	With toluene-4-sulfonic acid; 1-Nitroso-2-naphthol

Reference： [1]Current Patent Assignee: TOKUYAMA CORPORATION - JP2017/149650, 2017, A Location in patent: Paragraph 0193
[2]Current Patent Assignee: TOKUYAMA CORPORATION - JP2017/141212, 2017, A Location in patent: Paragraph 0191
[3]Arbusova,I.A. et al. [Journal of applied chemistry of the USSR, 1963, vol. 36, p. 1774 - 1777][Zhurnal Prikladnoi Khimii (Sankt-Peterburg, Russian Federation), 1963, vol. 36, # 8, p. 1833 - 1837]

2
[ 106-91-2 ]
[ 2761-09-3 ]

Yield	Reaction Conditions	Operation in experiment
98%	With chloroaluminium tetrahydroborate on poly(4-vinylpyridine) In ethanol for 7h; Heating;

Reference： [1]Tamami, Bahman; Lakouraj, M. Mansour; Yeganeh, Hamid [Journal of Chemical Research - Part S, 1997, # 9, p. 330 - 331]

3
[ 2761-09-3 ]
2-methyl-acrylic acid 3-(2,4,4,6,6-pentachloro-2λ⁵,4λ⁵,6λ⁵-[1,3,5,2,4,6]triazatriphosphinin-2-yloxy)-propyl ester [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine
	With pyridine; 2,2,4,4,6,6-hexachloro-1,3,5-triaza-2,4,6-triphosphorine; 4-methoxy-phenol In diethyl ether at 20℃; for 72h; Inert atmosphere; Molecular sieve;

Reference： [1]Allen, Christopher W.; Hayes, Robert F.; Myer, Charles N.; Freund, Amy S.; Kearney, Marie E. [Phosphorus, Sulfur and Silicon and the Related Elements, 1996, vol. 109, # 1-4, p. 79 - 82]
[2]Hayes, Robert F.; Allen, Christopher W. [Dalton Transactions, 2016, vol. 45, # 5, p. 2060 - 2068]

Yield	Reaction Conditions	Operation in experiment
		Representative hydroxyalkyl esters of acrylic or methacrylic acid include: 2-hydroxyethyl acrylate 2-hydroxyethyl methacrylate 3-hydroxypropyl acrylate 3-hydroxypropyl methacrylate 4-hydroxybutyl acrylate 4-hydroxybutyl methacrylate 2-hydroxy-1-methylethyl acrylate 2-hydroxy-1-methylethyl methacrylate,

5
[ 2761-09-3 ]
2-methylacrylic acid 2-carboxyethyl ester [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
47%	With jones reagent; 2,6-di-tert-butyl-4-methyl-phenol In acetone at 20℃; for 0.5h;

Reference： [1]Sibrian-Vazquez, Martha; Spivak, David A. [Journal of Organic Chemistry, 2003, vol. 68, # 25, p. 9604 - 9611]

6
[ 920-46-7 ]
[ 504-63-2 ]
[ 2761-09-3 ]

Yield	Reaction Conditions	Operation in experiment
45%	With trimethylamine In chloroform at 20℃; for 4h; Cooling;
39%	With triethylamine In tetrahydrofuran at 50℃; for 2h;
	With triethylamine In chloroform at 20℃; for 6h;

Reference： [1]Foster, Jeffrey C.; Varlas, Spyridon; Couturaud, Benoit; Jones, Joseph R.; Keogh, Robert; Mathers, Robert T.; O'Reilly, Rachel K. [Angewandte Chemie - International Edition, 2018, vol. 57, # 48, p. 15733 - 15737][Angew. Chem., 2018, vol. 130, p. 15959 - 15963,5]
[2]Sibrian-Vazquez, Martha; Spivak, David A. [Journal of Organic Chemistry, 2003, vol. 68, # 25, p. 9604 - 9611]
[3]Berchtold, Kathryn A.; Nie, Jun; Stansbury, Jeffrey W.; Hacioglu, Bilge; Beckel, Eric R.; Bowman, Christopher N. [Macromolecules, 2004, vol. 37, # 9, p. 3165 - 3179]

7
[ 2761-09-3 ]
polymer; monomer(s): 2-methylacrylic acid 3-hydroxypropyl ester [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,2-dimethoxy-2-phenylacetophenone at 25℃; UV-irradiation;

Reference： [1]Berchtold, Kathryn A.; Nie, Jun; Stansbury, Jeffrey W.; Hacioglu, Bilge; Beckel, Eric R.; Bowman, Christopher N. [Macromolecules, 2004, vol. 37, # 9, p. 3165 - 3179]

8
[ 674-82-8 ]
[ 2761-09-3 ]
3-(methacryloyloxy)propyl acetoacetate [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
60%	With triethylamine In dichloromethane at 0 - 20℃;

Reference： [1]Ivanovici, Sorin; Puchberger, Michael; Fric, Helmut; Kickelbick, Guido [Monatshefte fur Chemie, 2007, vol. 138, # 6, p. 529 - 539]

9
[ 2761-09-3 ]
[ 124-63-0 ]
C₈H₁₄O₅S [ No CAS ]

Reference： [1]Current Patent Assignee: FUJIFILM HOLDINGS CORP. - EP1174411, 2002, A2 Location in patent: Example 6

10
[ 100-42-5 ]
[ 868-77-9 ]
[ 2761-09-3 ]
[ 3066-71-5 ]
[ 79-10-7 ]
[ 97-88-1 ]
None [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	at 140℃; for 6.5h;	1 Preparation Example 1; The preparation of a methacrylate copolymer (A) A laboratory reactor with a useful volume of 4 l, equipped with a stirrer, two dropping funnels for the monomer mixture and initiator solution respectively, a nitrogen inlet pipe, thermometer, and reflux condenser, was charged with 601 g of an aromatic hydrocarbons fraction having a boiling range from 158° C. to 172° C. The solvent was heated to 140° C. When 140° C. had been reached, a monomer mixture of 225.4 g of styrene, 169 g of n-butyl methacrylate, 293 g of cyclohexyl acrylate, 225.4 g of hydroxypropyl methacrylate, 202.8 g of 2-hydroxyethyl methacrylate and 11.2 g of acrylic acid was metered into the reactor at a uniform rate over the course of 4 hours and an initiator solution of 112.6 g of t-butyl perethylhexanoate in 40 g of the aromatic solvent described was metered into the reactor at a uniform rate over the course of 4.5 hours. The metering of the monomer mixture and of the initiator solution was commenced simultaneously. After the end of the initiator feed the reaction mixture was held at 140° C. for 2 hours more, then diluted with 119.6 g of the aromatic solvent described, and subsequently cooled. The resulting polymer solution had a solids content of 60% by weight (determined in a forced-air oven, 1 h at 130° C.). The methacrylate copolymer had a hydroxyl number of 156 mg KOH/g, an acid number of 10 mg KOH/g, a number-average molecular weight of 1,700, and a glass transition temperature of +65° C.

Reference： [1]Current Patent Assignee: BASF SE - US2006/173120, 2006, A1 Location in patent: Page/Page column 10

11
[ 108-55-4 ]
[ 2761-09-3 ]
HPGM [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,6-di-tert-butyl-4-methyl-phenol; N-benzyl-N,N,N-triethylammonium chloride at 40 - 100℃; for 9h;	1 Synthesis Example 1: HPGM; Glutaric anhydride (22.8 g), hydroxypropylmethacrylate (28.8 g), butylated hydroxytoluene (BHT) (0.05 g), and benzyltriethylammonium chloride (TBAC, 0.05 g) were warmed and stirred in a closed flask to 400C until a homogenous liquid was obtained. The temperature was then raised to 1000C for 9 hours. After this time an FTIR spectrum of the mixture had only a very small peak due to the anhydride, and showed that the anhydride had therefore essentially completely reacted. A colourless clear liquid was obtained and was used without further purification. When applied to moistened pH indicator sticks (Machery-Nagel pH-Fix 0.0-6.0) a pH of 2.5 was indicated.

Reference： [1]Current Patent Assignee: DENTSPLY SIRONA INC - WO2006/84769, 2006, A1 Location in patent: Page/Page column 15

12
[ 80-62-6 ]
[ 504-63-2 ]
[ 2761-09-3 ]
[ 1188-09-6 ]

Yield	Reaction Conditions	Operation in experiment
	With 4-methoxy-phenol for 6h; Heating / reflux;	1 In an apparatus equipped with a 1-liter three-necked flask with mechanical stirrer, air inlet and top-mounted packed column (30 cm long, packed with 6 mm Raschig rings) as well as column head and reflux divider there were placed 67.5 g of 1,3-propanediol and 532 g of methyl methacrylate (MMA). To prevent undesired polymerization, 500 ppm of hydroquinone monomethyl ether was added. While air was being based in, the reaction mixture was heated to boiling. A resulting MMA-water azeotrope, which formed because of the use of moist starting materials, was distilled off until the head temperature stabilized (at about 100° C.) and clear MMA was passing over. The reaction mixture was cooled to about 90° C., and the MMA distilled off as an azeotrope was replaced by fresh. 6 g (1% of the relative weight of the reagents) of zirconium acelylacetonate was added to the mixture. The reaction mixture was then reheated to boiling, and the MMA methanol azeotrope formed was removed from the reaction mixture by distillation. In the process the head temperature rose from 65 to about 99° C., ultimately reaching the boiling point of pure MMA. After 6 hours the reaction had ceased. At that point in time only pure MMA was still passing over. The reaction mixture was cooled, after which 25 ml of 10% phosphoric acid (aqueous solution) was added to the mixture, whereupon the zirconium catalyst precipitated out. The formed precipitate was separated by filtration, and excess MMA was removed from the mixture under vacuum. The mixture was then analyzed by gas chromatography. The yield was 140 g. According to GC analysis, the end product contained 94.2% of 1,3-propanediol dimethacrylate, 5.2% of 1,3-propanediol monomethacrylate and 0.2% of 1,3-propanediol.

Reference： [1]Current Patent Assignee: ADVENT INTERNATIONAL CORPORATION; Roehm (in: Advent International) - US6639099, 2003, B1 Location in patent: Page/Page column 5-6

13
[ 364079-15-2 ]
[ 2761-09-3 ]
C₉₂H₁₁₀O₂₄ [ No CAS ]
C₉₂H₁₁₀O₂₄ [ No CAS ]
C₉₂H₁₁₀O₂₄ [ No CAS ]
C₅₈H₇₄O₁₆ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	Stage #1: sebacoyl chloride; bis 1,4 [4'-hydroxybenzoyloxy] t-butylphenylene With pyridine In dichloromethane for 6h; Stage #2: 2-methylacrylic acid 3-hydroxypropyl ester In dichloromethane for 6h;	20 71.40 g (0.3000 mole) of sebacoyl chloride was dissolved in 500 ml of dry methylene chloride in a one-liter flask. 8.13 g (0.0200 mole) of 1,4 bis(4'-hydroxybenzoyloxy)t-butylphenylene and 3.16 g (0.0400 mole) of pyridine were added to the flask and stirred under nitrogen for 6 hours.The solvent was vacuum-evaporated and the material taken up into 500 ml of hexane to extract out the excess sebacoyl chloride. The remaining material was dissolved in 500 ml of dry methylene chloride. 15.61 g (0.1200 mole) of hydroxypropyl methacrylate and 18.91 g (0.1200 mole) of pyridine were added to the flask and stirred to 6 hours under nitrogen.The solvent was vacuum-evaporated and the material taken up into 500 ml of ethyl ether. The amine hydrochloride salts precipitated out of the ether and were filtered off. The ethyl ether layer was stirred 5 times with 10 g with basic alumina to remove sebacic acid end groups. The remaining material was found to be 10/1 monomer to dimer that consisted of entirely primary HPMA addition.Methanol extraction of the mixture yielded the pure monomer, a low viscosity clear fluid with Tn→I=16° C. The remaining thick, white fluid dimer showed Tn→I=81-83° C.

Reference： [1]Current Patent Assignee: SOUTHWEST RESEARCH INSTITUTE INC - US7098359, 2006, B2 Location in patent: Page/Page column 34

14
[ 2761-09-3 ]
[ 107-13-1 ]
None [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,2'-azobis(isobutyronitrile) In ethanol at 60 - 70℃; for 0.333333h;	2 10 ml of HPMA monomer 1 are poured into a 1 liter two-necked round-bottomed flask. 50 mg of AIBN (copolymer-ization-initiating agent) and 30 ml of absolute ethanol, and optionally the amount indicated above of comonomer 2 (AN, TBA or AAMA) are then added. A condensing column is placed on the round-bottomed flask, a waterbath makes it possible to regulate the temperature of the reaction mixture. An ovoid stirrer makes it possible to homogenize the solution. Argon is bubbled in for 10 minutes in order to eliminate the O2 molecules that could take up the free radicals and impair the polymerization reaction. When the bubbling is complete, the waterbath is brought to a temperature of between 60 and 70° C. The stirring is maintained for 10 minutes, and then 20 ml of ethanol are subsequently added in order to decrease the viscosity of the mixture. Two successive precipitations are then carried out. First precipitation: the reaction mixture is poured into a 5 liter beaker containing 4 liters of deionized water. Upon contact with the water, the reaction mixture precipitates and forms a polymer cloud. This cloud is then wound around a glass stirrer in the form of an anchor and removed from the beaker. The polymer is then redissolved in 500 ml of absolute ethanol at a temperature of 70° C. in order to wash from it the impurities that could remain (monomers, initiating agent). The polymer solution is then cooled. Second precipitation: the solution is then precipitated a second time as described above. The precipitated polymer recovered is then dried in an oven at a temperature of approximately 50° C. for several hours, and then in a vacuum oven for approximately 12 hours. When the polymer is completely dry, it is broken up into small pieces manually and packaged in hermetically sealed plastic bottles.

Reference： [1]Current Patent Assignee: ASSISTANCE PUBLIQUE - HÔPITAUX DE PARIS; UNIVERSITE PARIS XI - US2006/210635, 2006, A1 Location in patent: Page/Page column 5-6

15
[ 2761-09-3 ]
[ 21282-97-3 ]
None [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,2'-azobis(isobutyronitrile) In ethanol at 60 - 70℃; for 0.333333h;	2 10 ml of HPMA monomer 1 are poured into a 1 liter two-necked round-bottomed flask. 50 mg of AIBN (copolymer-ization-initiating agent) and 30 ml of absolute ethanol, and optionally the amount indicated above of comonomer 2 (AN, TBA or AAMA) are then added. A condensing column is placed on the round-bottomed flask, a waterbath makes it possible to regulate the temperature of the reaction mixture. An ovoid stirrer makes it possible to homogenize the solution. Argon is bubbled in for 10 minutes in order to eliminate the O2 molecules that could take up the free radicals and impair the polymerization reaction. When the bubbling is complete, the waterbath is brought to a temperature of between 60 and 70° C. The stirring is maintained for 10 minutes, and then 20 ml of ethanol are subsequently added in order to decrease the viscosity of the mixture. Two successive precipitations are then carried out. First precipitation: the reaction mixture is poured into a 5 liter beaker containing 4 liters of deionized water. Upon contact with the water, the reaction mixture precipitates and forms a polymer cloud. This cloud is then wound around a glass stirrer in the form of an anchor and removed from the beaker. The polymer is then redissolved in 500 ml of absolute ethanol at a temperature of 70° C. in order to wash from it the impurities that could remain (monomers, initiating agent). The polymer solution is then cooled. Second precipitation: the solution is then precipitated a second time as described above. The precipitated polymer recovered is then dried in an oven at a temperature of approximately 50° C. for several hours, and then in a vacuum oven for approximately 12 hours. When the polymer is completely dry, it is broken up into small pieces manually and packaged in hermetically sealed plastic bottles.

Reference： [1]Current Patent Assignee: ASSISTANCE PUBLIQUE - HÔPITAUX DE PARIS; UNIVERSITE PARIS XI - US2006/210635, 2006, A1 Location in patent: Page/Page column 5-6

16
[ 107-58-4 ]
[ 2761-09-3 ]
None [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,2'-azobis(isobutyronitrile) In ethanol at 60 - 70℃; for 0.333333h;	2 10 ml of HPMA monomer 1 are poured into a 1 liter two-necked round-bottomed flask. 50 mg of AIBN (copolymer-ization-initiating agent) and 30 ml of absolute ethanol, and optionally the amount indicated above of comonomer 2 (AN, TBA or AAMA) are then added. A condensing column is placed on the round-bottomed flask, a waterbath makes it possible to regulate the temperature of the reaction mixture. An ovoid stirrer makes it possible to homogenize the solution. Argon is bubbled in for 10 minutes in order to eliminate the O2 molecules that could take up the free radicals and impair the polymerization reaction. When the bubbling is complete, the waterbath is brought to a temperature of between 60 and 70° C. The stirring is maintained for 10 minutes, and then 20 ml of ethanol are subsequently added in order to decrease the viscosity of the mixture. Two successive precipitations are then carried out. First precipitation: the reaction mixture is poured into a 5 liter beaker containing 4 liters of deionized water. Upon contact with the water, the reaction mixture precipitates and forms a polymer cloud. This cloud is then wound around a glass stirrer in the form of an anchor and removed from the beaker. The polymer is then redissolved in 500 ml of absolute ethanol at a temperature of 70° C. in order to wash from it the impurities that could remain (monomers, initiating agent). The polymer solution is then cooled. Second precipitation: the solution is then precipitated a second time as described above. The precipitated polymer recovered is then dried in an oven at a temperature of approximately 50° C. for several hours, and then in a vacuum oven for approximately 12 hours. When the polymer is completely dry, it is broken up into small pieces manually and packaged in hermetically sealed plastic bottles.

Reference： [1]Current Patent Assignee: ASSISTANCE PUBLIQUE - HÔPITAUX DE PARIS; UNIVERSITE PARIS XI - US2006/210635, 2006, A1 Location in patent: Page/Page column 5-6

17
[ 2761-09-3 ]
[ 814-49-3 ]
[ 99993-26-7 ]

Yield	Reaction Conditions	Operation in experiment
71%	With pyridine; triethylamine In dichloromethane at 0 - 20℃; Inert atmosphere;

Reference： [1]Location in patent: experimental part Francova, Denisa; Kickelbick, Guido [Monatshefte fur Chemie, 2009, vol. 140, # 4, p. 413 - 422]

18
[ 5536-61-8 ]
[ 627-30-5 ]
[ 2761-09-3 ]

Reference： [1]Monatshefte fur Chemie,2009,vol. 140,p. 413 - 422

19
[ 80-62-6 ]
[ 504-63-2 ]
[ 2761-09-3 ]

Yield	Reaction Conditions	Operation in experiment
	With Novozyme 435 In tert-Amyl alcohol at 50℃; for 120h; Inert atmosphere; Molecular sieve; Enzymatic reaction;
25 %Chromat.	With [2,2]bipyridinyl; [Zn(2,2,6,6-tetramethyl-3,5-heptanedione)(OMe)(MeOH)]₄ In toluene at 85℃; for 3h; chemoselective reaction;

Reference： [1]Location in patent: experimental part Popescu, Dragos; Hoogenboom, Richard; Keul, Helmut; Moeller, Martin [Journal of Molecular Catalysis B: Enzymatic, 2010, vol. 62, # 1, p. 80 - 89]
[2]Kato, Taito; Akebi, Shin-Ya; Nagae, Haruki; Yonehara, Koji; Oku, Tomoharu; Mashima, Kazushi [Catalysis science and technology, 2021, vol. 11, # 21, p. 6975 - 6986]

20
[ 2761-09-3 ]
[ 16926-87-7 ]
[ 5124-30-1 ]
C₃₅H₅₀N₂O₉ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	With 2,6-di-tert-butyl-4-methyl-phenol; dibutyltin dilaurate at 50℃; Inert atmosphere;	4.22 22. Synthesis of PDCHDMA 22. Synthesis of PDCHDMA (0220) (0221) In a two neck flask under nitrogen atmosphere were mixed together 13.00 g (0.050 mol) of dicyclohexylmethane-4,4′-diisocyanate, 7.28 g (0.051 mol) of hydroxypropyl methacrylate (1.02 equivalents), 11.93 g (0.051 mol) of (V) (1.02 equivalents), and 30 mg of BHT. To continue 10 mg of DBTDL were added. Reaction mixture was stirred at 50° C. until next day. Reaction product was isolated as viscous oil and can be used without further purification

Reference： [1]Current Patent Assignee: SEPTODONT INC - US8513326, 2013, B2 Location in patent: Page/Page column 40; 41; 42

21
[ 2761-09-3 ]
C₁₉H₂₁FO₃ [ No CAS ]
C₂₆H₃₁FO₅ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
19 g	With di-isopropyl azodicarboxylate; triphenylphosphine In tetrahydrofuran at 20℃; for 5h; Cooling with ice;	6 The compound 17.0g (0.0537 mol) expressed with a formula (I-6-4) by the reaction containerprovided with the dropping funnel, the compound 11.0g (0.0698 mol) denoted by a formula (I-6-5), 16.9 g (0.0644 mol) of triphenyl phosphine, and 200 mL of tetrahydrofurans were added.13.0 g (0.0644 mol) of diisopropyl azodicarboxylate was dropped icecooling. After agitating ata room temperature for 5 hours, column chromatography (silica gel) refined and it obtainedthe compound 19.0g (0.0429 mol) denoted by a formula (I-6-6).

Reference： [1]Current Patent Assignee: DIC CORP. - JP2015/110531, 2015, A Location in patent: Paragraph 0141; 0145

22
[ 2761-09-3 ]
[ 15396-00-6 ]
C₁₄H₂₇NO₇Si [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
75%	With 1,4-diaza-bicyclo[2.2.2]octane at 80℃;	21.2 Example 21 (2) In the presence of a stirrer,thermometer,A reflux condenser was charged with 21.63 g (0.15 mol) of hydroxypropyl methacrylate, and 0.06 g of triethylenediamine was added dropwise. The mixture was stirred well,Then, 20.53 g (0.1 mol) of γ-isocyanatopropyltrimethoxysilane was dropwise added through a constant-pressure dropping funnel, the dropping speed was controlled,The reaction temperature was maintained at 80 ° C,Until the end of the reaction.Washed twice with petroleum ether. Yield 75%.

Reference： [1]Current Patent Assignee: BEIJING UNIVERSITY OF CHEMICAL TECHNOLOGY - CN106279241, 2017, A Location in patent: Paragraph 0093; 0094

23
[ 2761-09-3 ]
[ 7158-32-9 ]
C₂₈H₃₀O₉ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
76%	With dmap; triethylamine; In dichloromethane; at 20℃; for 1h;	Next, a solution containing 3.0 g (0.01 mol) of the acid chloride (A), 70 ml of methylene chloride and 0.001 g of di-tertbutylmethylphenol in a separate glass container was added to this solution while stirring , A solution prepared by dissolving 3.2 g (0.022 mol) of the above-mentioned 3-hydroxypropyl methacrylate, 2.0 g (0.02 mol) of triethylamine and 0.025 g (0.0002 mol) of 4-dimethylaminopyridine in 10 ml of methylene chloride It slowly dripped over 1 hour. The solution obtained after the dropwise addition was stirred at room temperature for 1 hour, then water was added and the solvent was removed using a rotary evaporator. The residue obtained after removing the solvent was dissolved in 100 ml of toluene, washed with 0.5 N hydrochloric acid solution, washed with saturated brine, dried over magnesium sulfate and filtered. The resulting filtrate was concentrated again on a rotary evaporator, and the concentrate was further dried under vacuum to obtain 4-DPEHP (yield 4.1 g, yield 76%, HPLC purity 97%). The data of the 1 H NMR spectrum of the obtained 4-DPEHB
76%	With dmap; 2,6-di-tert-butyl-4-methyl-phenol; triethylamine; In dichloromethane; at 20℃; for 2h;	next,In a separate glass container, 3.0 g (0.01 mol) of the acid chloride (A), 70 ml of methylene chloride,Di-tert-butyl methyl phenol 0.001 gWhile stirring the solution,To this solution,The above 3-hydroxypropyl methacrylate3.2 g (0.022 mol),2.0 g (0.02 mol) of triethylamine,And 0.025 g (0.0002 mol) of 4-dimethylaminopyridine in 10 ml of methylene chloride over 1 hour,Was slowly added dropwise. After completion of the dropwise addition,After stirring at room temperature for 1 hour,Water was added and, using a rotary evaporator,The solvent was removed. The residue obtained after removing the solvent was dissolved in 100 ml of toluene, washed with 0.5 N hydrochloric acid solution, washed with saturated brine, dried over magnesium sulfate and filtered. The resulting filtrate was concentrated again on a rotary evaporator, and the concentrate was further vacuum-dried to obtain 4-DPEHP (yield 4.1 g, yield 76%, HPLC purity 97%).Incidentally,

Reference： [1]Patent: JP2017/149650,2017,A .Location in patent: Paragraph 0193; 0194
[2]Patent: JP2017/141212,2017,A .Location in patent: Paragraph 0192

24
[ 2761-09-3 ]
C₁₄H₂₃O₈P [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
71%	With water; triethylamine; trichlorophosphate In tetrahydrofuran at 20℃; for 5h; Cooling with ice;	Synthesis of DMPP Into 100 ml of dehydrated tetrahydrofuran were added 30.7 g (0.2 mol)Of phosphoryl chloride was dissolved, and the solution was cooled in an ice bath,57.7 g (0.4 mol) of 3-methacryloyloxypropanol and 40.5 g (0.4 mol) of triethylamine were added dropwise over 1 hour.After completion of the dropwise addition, the mixture was further stirred at room temperature for 3 hours,3.6 g (0.2 mol) of water and 20.3 g (0.2 mol) of triethylamine were added dropwise, and the mixture was stirred for 1 hour.After stirring, 100 ml of 0.5 N hydrochloric acid was added,And extracted three times with 50 ml of diethyl ether. Further, the diethyl ether layer was washed once with 50 ml of 0.5 N hydrochloric acid and twice with distilled water,And dried on granular silica gel. After drying,Diethyl ether was distilled off with a rotary evaporator,The residue was purified by silica gel column chromatography,DMPP (49.7 g, yield 71%) was obtained. Incidentally,The 1 H NMR spectrum data of the obtained DMPP is shown in FIG.

Reference： [1]Current Patent Assignee: TOKUYAMA CORPORATION - JP2018/65831, 2018, A Location in patent: Paragraph 0071

25
[ 760-93-0 ]
[ 504-63-2 ]
[ 2761-09-3 ]

Yield	Reaction Conditions	Operation in experiment
92%	With triethylamine In chloroform at 30℃; Inert atmosphere;

Reference： [1]Lai, Jinping; Abune, Lidya; Zhao, Nan; Wang, Yong [Angewandte Chemie - International Edition, 2019, vol. 58, # 9, p. 2820 - 2825][Angew. Chem., 2019, vol. 131, # 9, p. 2846 - 2851,6]

26
[ 2761-09-3 ]
3-(2-hydroxyethyl)-4-nitrobenzaldehyde [ No CAS ]
C₂₃H₃₁NO₉ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
48%	With 2,6-di-tert-butyl-4-methyl-phenol; pyridinium p-toluenesulfonate In toluene Molecular sieve; Inert atmosphere; Reflux;

27
[ 2761-09-3 ]
[ 31643-49-9 ]
C₁₅H₁₄N₂O₃ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
64%	With potassium carbonate In dimethyl sulfoxide at 15℃; for 24h; Inert atmosphere;	2 Example 2 To the three-necked flask which was purged with nitrogen gas, 21.2 mL of an acrylate monomer HEMA having a hydroxyl group structure as shown in FIG. 1 , 10 g of 4-nitrophthalic acid NPh, and 20 g of potassium carbonate were sequentially added.N,N-dimethylacetamide 200 mL.The reaction was carried out under a nitrogen atmosphere at room temperature (25 ° C) for 48 hours, the heating was stopped, and the product was poured into a 5% by mass aqueous NaOH solution. After filtration, the cake was collected and washed until neutral. After drying at 50 ° C for 24 hours, the mixture was subjected to column chromatography using chloroform as an eluent, and the main components were collected. The product was collected by spin-drying using a rotary evaporator and recrystallized from tetrahydrofuran in a ratio of 1:10 g/mL. After filtration and drying in vacuo, the product was obtained in a yield of 71%.

Reference： [1]Current Patent Assignee: DALIAN UNIVERSITY OF TECHNOLOGY; DELFT UNIVERSITY OF TECHNOLOGY - CN109704989, 2019, A Location in patent: Paragraph 0026-0028

28
[ 2761-09-3 ]
C₅₂H₇₂O₄ [ No CAS ]
C₅₉H₈₂O₆ [ No CAS ]
C₆₆H₉₂O₈ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
1: 24.5% 2: 32.4%	Stage #1: 2-methylacrylic acid 3-hydroxypropyl ester; C₅₂H₇₂O₄ With triphenylphosphine In tetrahydrofuran Stage #2: With di-isopropyl azodicarboxylate In tetrahydrofuran at 20℃; for 10.5h; Cooling with ice;	21 Example 7 General procedure: In a 100-mL four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, 2.00 g (2.014 mmol) of the compound obtained in Synthesis Example 7, 7.26 g of tetrahydrofuran, 1.056 g (4.027 mmol) of triphenylphosphine, and 0.347 g (4.027 mmol) of methacrylic acid were added and stirred. A clear pale yellow solution. Next, in an ice bath, 0.905 g (4.027 mmol) of diisopropyl azodicarboxylate was added dropwise over 30 minutes. A clear pale yellow solution. Stirring was performed at room temperature for 10 hours. Hexane was added to the reaction solution to remove by-products, such as triphenylphosphine, by precipitation, and thereafter chloroform extraction was carried out. The extracts were washed with water and saturated brine and subsequently dried with magnesium sulfate. The solvent was evaporated using an evaporator. An orange viscous liquid was purified by column chromatography (developing solvent: n-hexane:acetone=90:10). Thus, a compound (7-1), two compounds (7-2) and (7-3), and a compound (7-4), which are represented by the structural formulae below, were obtained. The compound (7-1) contained, as R5's, three structural moieties (A) and one structural moiety (B). The compounds (7-2) and (7-3) each contained two structural moieties (A) and two structural moieties (B). The compound (7-4) contained one structural moiety (A) and three structural moieties (B). The compounds were dried under vacuum (at 60° C. for 6 hours or more). The compounds were in respective amounts of 0.765 g, 0.321 g, 0.287 g, and 0.101 g, with the respective yields being 35.8%, 14.1%, 12.6%, and 4.2%.

Reference： [1]Current Patent Assignee: DIC CORP. - US2021/198178, 2021, A1 Location in patent: Paragraph 0145; 0166

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P378
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P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
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P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
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H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
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H242	Heating may cause a fire
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H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
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Health hazards
Code	Phrase
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H302	Harmful if swallowed
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H316	Causes mild skin irritation
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Environmental hazards
Code	Phrase
H400	Very toxic to aquatic life
H401	Toxic to aquatic life
H402	Harmful to aquatic life
H410	Very toxic to aquatic life with long-lasting effects
H411	Toxic to aquatic life with long-lasting effects
H412	Harmful to aquatic life with long-lasting effects
H413	May cause long-lasting harmful effects to aquatic life
H420	Harms public health and the environment by destroying ozone in the upper atmosphere

[ CAS No. 2761-09-3 ] {[proInfo.proName]}

Quality Control of [ 2761-09-3 ]

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Product Details of [ 2761-09-3 ]

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Application In Synthesis of [ 2761-09-3 ]

[ 2761-09-3 ] Synthesis Path-Downstream 1~28

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