[ CAS No. 3424-43-9 ] {[proInfo.proName]}

Name: 3424-43-9|Ethyl 2-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate|98%
Brand: Ambeed
SKU: A393416
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Quality Control of [ 3424-43-9 ]

COA NMR CNMR HPLC LC-MS

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SDS Specification

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Product Details of [ 3424-43-9 ]

CAS No. :	3424-43-9	MDL No. :	MFCD01871481
Formula :	C₉H₁₁NO₃	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	UEZSEPUDNLUVNJ-UHFFFAOYSA-N
M.W :	181.19	Pubchem ID :	3299500
Synonyms :

Calculated chemistry of [ 3424-43-9 ]

Physicochemical Properties

Num. heavy atoms :	13
Num. arom. heavy atoms :	6
Fraction Csp3 :	0.33
Num. rotatable bonds :	3
Num. H-bond acceptors :	3.0
Num. H-bond donors :	1.0
Molar Refractivity :	48.12
TPSA :	59.16 Å²

Pharmacokinetics

GI absorption :	High
BBB permeant :	Yes
P-gp substrate :	No
CYP1A2 inhibitor :	No
CYP2C19 inhibitor :	No
CYP2C9 inhibitor :	No
CYP2D6 inhibitor :	No
CYP3A4 inhibitor :	No
Log Kp (skin permeation) :	-7.04 cm/s

Lipophilicity

Log Po/w (iLOGP) :	1.88
Log Po/w (XLOGP3) :	0.52
Log Po/w (WLOGP) :	0.86
Log Po/w (MLOGP) :	0.85
Log Po/w (SILICOS-IT) :	2.14
Consensus Log Po/w :	1.25

Druglikeness

Lipinski :	0.0
Ghose :	None
Veber :	0.0
Egan :	0.0
Muegge :	1.0
Bioavailability Score :	0.55

Water Solubility

Log S (ESOL) :	-1.43
Solubility :	6.66 mg/ml ; 0.0368 mol/l
Class :	Very soluble
Log S (Ali) :	-1.33
Solubility :	8.41 mg/ml ; 0.0464 mol/l
Class :	Very soluble
Log S (SILICOS-IT) :	-2.8
Solubility :	0.287 mg/ml ; 0.00158 mol/l
Class :	Soluble

Medicinal Chemistry

PAINS :	0.0 alert
Brenk :	0.0 alert
Leadlikeness :	1.0
Synthetic accessibility :	1.87

Safety of [ 3424-43-9 ]

Signal Word:	Warning	Class:	N/A
Precautionary Statements:	P261-P280-P301+P312-P302+P352-P305+P351+P338	UN#:	N/A
Hazard Statements:	H302-H315-H320-H335	Packing Group:	N/A
GHS Pictogram:

Application In Synthesis of [ 3424-43-9 ]

* 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.

Upstream synthesis route of [ 3424-43-9 ]
Downstream synthetic route of [ 3424-43-9 ]

[ 3424-43-9 ] Synthesis Path-Upstream 1~1

1
[ 3424-43-9 ]
[ 3279-76-3 ]

Reference： [1] Journal of Organic Chemistry, 1954, vol. 19, p. 183,191
[2] Journal of Organic Chemistry, 1954, vol. 19, p. 183,191

[ 3424-43-9 ] Synthesis Path-Downstream 1~58

1
[ 3424-43-9 ]
[ 31163-12-9 ]

Yield	Reaction Conditions	Operation in experiment
89%	With trichlorophosphate In N,N-dimethyl-formamide at 120℃; for 2h; Inert atmosphere;	69 ethyl 6-chloro-2-methylnicotinate (4): A solution of ethyl 6-hydroxy-2-methylnicotinate compound 3 (8.11 g, 44.6 mmol) andphosphorous oxychloride (20.0 g, 130 mmol) was stirred under nitrogen atmosphere at 120 °C for 2 hours. After cooling, the mixture was poured into ice water, basified with 8 M NaOH aqueoussolution, and extracted with EtOAc. The extract was washed with brine, dried over anhydrousNa2SO4 and concentrated under reduced pressure to obtain crude product, which was purified by silica gel column chromatography eluting with 30% EtOAc /PE to afford compound 4 (7.88 g,89%) as a colorless oil. LC-MS: m/z =200.0 [M+H]
	With trichlorophosphate at 130℃;
	With trichlorophosphate at 140℃; for 1h;	1.4; 2.4; 3.4; 4.4 76g of intermediate product C was mixed with 300mL of POC13 solution and heated to 140°C for 1 hour. After the reaction,The mixed product obtained by the reaction was evaporated to remove excess POC13, and then added to the saturated NaHC03 solution and fully stirredAfter mixing, add 450mL ethyl acetate for extraction, then use anhydrous Na2S04 to dry and concentrate to dryness to obtain 88g intermediate productD.

58.7 g

With trichlorophosphate for 2h; Reflux; Inert atmosphere;

185.4 Step 4: The crude 184-4 (57.8 g) was dissolved in phosphorus oxychloride (196.26 g, 1.28 mol), heated to reflux and stirred for 2h under nitrogen. TLC showed that the raw material was completely reacted. The reaction solution was cooled to room temperature and concentrated. The residue was poured into ice water, alkalized with 8M NaOH aqueous solution, and extracted with ethyl acetate. The combined organic phase was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated. The crude was purified by silica gel column chromatography to obtain 184-5 (58.7 g) as a white solid. LC-MS: 200.1 [M+1]+.

Reference： [1]Current Patent Assignee: ABBVIE INC - WO2016/44770, 2016, A1 Location in patent: Page/Page column 605
[2]Ramirez; Paul [Journal of Organic Chemistry, 1954, vol. 19, p. 183,191]
[3]Current Patent Assignee: SUZHOU CHIEN SHIUNG INST TECH - CN111499574, 2020, A Location in patent: Paragraph 0012; 0040-0041; 0055-0058; 0080; 0094-0097; 0119
[4]Current Patent Assignee: Shanghai Institute of Materia Medica (in: CAS); CHINESE ACADEMY OF SCIENCES - EP3782995, 2021, A1 Location in patent: Paragraph 0659; 0663

2
[ 141-52-6 ]
[ 95387-37-4 ]
[ 3424-43-9 ]

Reference： [1]Journal of Organic Chemistry,1985,vol. 50,p. 1512 - 1516

3
[ 141-52-6 ]
[ 95387-40-9 ]
[ 3424-43-9 ]
[ 95387-42-1 ]

Reference： [1]Journal of Organic Chemistry,1985,vol. 50,p. 1512 - 1516

4
[ 67-56-1 ]
[ 50-00-0 ]
[ 3424-43-9 ]
[ 74-88-4 ]
[ 123435-97-2 ]

Reference： [1]Tetrahedron Letters,1989,vol. 30,p. 2089 - 2090

5
[ 4027-39-8 ]
[ 3424-43-9 ]

Yield	Reaction Conditions	Operation in experiment
62%	With 2,3-dicyano-5,6-dichloro-p-benzoquinone; In 1,4-dioxane; for 5.0h;Heating / reflux;	Ethyl 2-methyl-6-oxo-l,4,5,6-tetrahydropyridine-3-carboxylate (2g, 10.93mmol) and DDQ (5.21g, 22.95mmol) in 1,4-dioxaxne (110ml) were heated under reflux for 5h. The residue obtained after evaporation of solvent under reduced pressure was partitioned between DCM and water and washed with sat. sodium hydrogen carbonate solution. The aqueous layer was extracted with DCM twice. The organics were combined, washed with brine, dried and the solvent was evaporated to give a solid which was purified by chromatography eluting with MeOH:DCM (1 :99 to 4:96). Insoluble material in DCM and MeOH, prior to purification, was filtered off to give pure product. The product obtained after purification was dissolved in DCM and passed through a pre-equilibrated neutral alumina column, eluting with DCM, then 5% MeOH:DCM. Re-evaporation of solvent gave the title compound as a solid which was dried in vac oven overnight at 50C (1.23g, 62%). NMR (400MHz): 1.28 (t, 3H), 2.53 (s, 3H), 4.21 (q, 2H), 6.21 (d, IH), 7.82 (d, IH), 12.00 (s, IH); m/z 182. As an alternative to the above, the reaction mixture may be diluted with DCM and passed through a pre-equilibrated neutral alumina column, eluting with DCM, then MeOH. EPO <DP n="62"/>Chromatography on silica gel, then neutral alumina column eluting with DCM gave the product.

Reference： [1]Patent: WO2006/95159,2006,A1 .Location in patent: Page/Page column 60-61
[2]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

6
[ 3424-43-9 ]
[ 74-88-4 ]
[ 173261-76-2 ]

Yield	Reaction Conditions	Operation in experiment
75%	With silver carbonate; at 50℃; for 16.0h;	: To a suspension of ethyl2-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate (0.2 g, 1.06 mmol) and Ag2CO3(0.44 g, 1.59 mmol) was added methyl iodide (0.3 mL, 4.24 mmol)and the reaction mixture was heated at 50 C for 16 h. The reaction mixture wascooled to room temperature, filtered and concentrated. The crude residue waspurified by Combiflash with 20% EtOAc in Hexane to afford the title compound asoff-white solid (0.25 g, 75%). 1H NMR (DMSO-d6, 400 MHz) δ1.37 (t, J = 7.2 Hz, 3H), 2.75 (s,3H), 3.96 (s, 3H), 4.33 (q, J = 7.2Hz, 2H), 6.57 (d, J = 8.4 Hz, 1H),8.11 (d, J = 8.8 Hz, 1H); MS (ESI) m/z196.1 (M+H)+.

Reference： [1]Bioorganic and Medicinal Chemistry Letters,2018,vol. 28,p. 922 - 925
[2]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

8
[ 4027-39-8 ]
[ 546-67-8 ]
2-acetoxymethyl-6-oxo-1,6-dihydro-pyridine-3-carboxylic acid ethyl ester [ No CAS ]
2-acetoxymethyl-6-oxo-1,4,5,6-tetrahydro-pyridine-3-carboxylic acid ethyl ester [ No CAS ]
[ 3424-43-9 ]

Reference： [1]Synthetic Communications,2005,vol. 35,p. 2993 - 3001

9
[ 6296-99-7 ]
[ 141-97-9 ]
[ 3424-43-9 ]

Reference： [1]Tetrahedron,2006,vol. 62,p. 6222 - 6227
[2]Synthetic Communications,2005,vol. 35,p. 2993 - 3001

10
[ 141-97-9 ]
[ 100643-08-1 ]
[ 3424-43-9 ]

Reference： [1]Synthetic Communications,2005,vol. 35,p. 2993 - 3001

11
[ 3424-43-9 ]
1,6-dihydro-2-methyl-6-oxo-nicotinic acid [ No CAS ]

Reference： [1]Tetrahedron,2006,vol. 62,p. 6222 - 6227

12
[ 3424-43-9 ]
[ 919354-84-0 ]

Yield	Reaction Conditions	Operation in experiment
14%	With (bis-(2-methoxyethyl)amino)sulfur trufluoride; In acetonitrile;Heating / reflux;	Example 1; 25 Ethyl 6-(4-[(benzylsulfoϖyl)amino]carbonyl}piperidin-l-yl)-5-chloro-2- (difluoromethyl)nicotinate(a) Ethyl 2-(difluoromethyl)-6-oxo-l,6-dihydropyridine-3-carboxylate30 Ethyl 2-methyl-6-oxo-l,6-dihydropyridine-3-carboxylate (2.0 g, 11.04 mmol) ( Sobczak, A et al, Synth. Comrnun, VoL 35, No. 23, 2005, pρ2993-3001) was added to a solution of 2- methoxy-N-(2-merhoxyethyl)-N-(trifiuoro-λ4-sulfanyl)ethanamine (7.82 g, 22.08 mmol) in <n="86"/>85CH3CN under an atmosphere of nitrogen. The reaction was refluxed over night after which further 2-methoxy-N-(2-methoxyethyl)-N-(trifluoro-λ4-sulfanyl)ethanamine (2.73 g, 7.7 mmol) was added and the stirring was continued until all starting material was consumed. The reaction was diluted with diethyl ether, filtered to remove black solids, washed with5 water and NaHCO3 (aq,sat). Both phases were filtered again to remove more of black solids. The aqueous phase was extracted with diethyl ether (2 times) and the combined organic phase was dried (MgSO4), filtered and concentrated and slurried in diethyl ether to remove yellow impurities. Drying of the remaining white solid gave ethyl 2- (difluoromethyl)-6-oxo-l,6-dihydropyridine-3-carboxylate. Yield: 370 mg (14 %). io 1H NMR (400 MHz, CDCi) δ 1.38 (3H, t, J= 7.2 Hz), 4.36 (2H, q, J= 7.2 Hz), 6.69 (IH, d, J= 10 Hz), 7.56 (IH, t, J= 54 Hz), 7.99 (IH, d, J= 10 Hz).;

Reference： [1]Patent: WO2008/4946,2008,A1 .Location in patent: Page/Page column 84-85

13
[ 10444-33-4 ]
[ 3424-43-9 ]

Reference： [1]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

14
[ 3424-43-9 ]
[ 32383-10-1 ]

Reference： [1]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

15
[ 3424-43-9 ]
[ 173261-78-4 ]

Reference： [1]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

16
[ 3424-43-9 ]
[ 173261-77-3 ]

Reference： [1]Medicinal Chemistry Research,1995,vol. 5,p. 587 - 594

17
[ 23941-84-6 ]
[ 3424-43-9 ]

Reference： [1]Journal of Organic Chemistry,1985,vol. 50,p. 1512 - 1516

18
[ 3424-43-9 ]
[ 31163-12-9 ]

Yield	Reaction Conditions	Operation in experiment
94.7%		As shown in step 8-i of Scheme 8, according to the procedure of International Patent Application Publication No. WO2006/095159, a mixture of ethyl 2-methyl-6-oxo- 1 ,6- dihydropyridine-3-carboxylate (5.92 g, 32.6 mmol) in phosphorous oxychloride (45 mL) was heated at 90C for 1 hour. After cooling, the reaction mixture was concentrated under reduced pressure and ice water was added to the residue, followed by addition 28% ammonium hydroxide to adjust the pH to 7. The resulting white solid was collected by filtration, washed with ice water, and dried under high vacuum to give ethyl 6-chloro-2- methylnicotinate (Compound 2027, 6.18 g, 94.7% yield): ESMS (M+l) 200.19; 1H NMR (CDCls) δ 8.18 (d, J = 8.2 Hz, 1H), 7.27 (d, J = 8.2 Hz, 1H), 4.40 (q, J = 7.1 Hz, 2H), 2.84 (s, 3H), 1.42 (t, J = 7.4, 3H).
81%	With trichlorophosphate;Heating / reflux;	Ethyl 2-methyl-6-oxo-l,6-dihydropyridine-3-carboxylate (Method 2; 2.281g, 12.60mmol) and phosphorus oxychloride (50ml) were heated under reflux overnight. The oil obtained on evaporation of solvent was poured onto ice and solution neutralised with aq NH3. The resulting precipitate was filtered off, washed with water and air-dried, to give the title compound as a solid (2.32g, 81%). NMR (400MHz): 1.33 (t, 3H), 2.70 (s, 3H), 4.33 (q, 2H), 7.49 (d, IH), 8.21 (d, IH); m/z 200-202.

Reference： [1]Journal of Medicinal Chemistry,2018,vol. 61,p. 5245 - 5256
[2]Patent: WO2011/87776,2011,A1 .Location in patent: Page/Page column 62; 64
[3]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552
[4]Patent: WO2006/95159,2006,A1 .Location in patent: Page/Page column 3
[5]Journal of Medicinal Chemistry,2010,vol. 53,p. 3814 - 3830
[6]Patent: WO2018/140809,2018,A1 .Location in patent: Paragraph 00477

19
[ 3424-43-9 ]
[ 919354-64-6 ]

Yield	Reaction Conditions	Operation in experiment
52%	With N-chloro-succinimide; In N,N-dimethyl-formamide; at 20 - 100℃; for 1.5h;	Ethyl 2-methyl-6-oxo-l,6-dihydropyridine-3-carboxylate (2.00 g, 11.0 mmol), (Raileanu D., et. al. Tetrahedron , VoI 30 pp 623-32, 1974) was dissolved in DMF (35 mL) under a nitrogen atmosphere. NCS (1.53g, 11.5 mmol) taken upp in DMF (5.0 mL) at r.t. The reaction mixture was heated at 1000C for Ih. An additional amount of NCS (500mg, 3.8 mmol) was added and the reaction mixture was stirred for 0.5h. The reaction mixture was diluted with DCM were washed with water and brine once each. The aqueous phase was extracted with DCM twice and the combined organic phases were passed through a phase separator and the solvents were removed in vacuo. The crude product was purified by flash chromatography on silica (Biotage horizon)frst EtO Ac/heptane 1:1 followed by EtOAc to give ethyl 5-chloro-2-methyl-6-oxo- l,6-dihydropyridine-3-carboxylate as a yellow solid Yield=1.362g( 52%). 1H NMR (400 MHz, DMSO-d6) 5 1.37 (3H, 1, J= 7.3 Hz), 2.74 (3H, s), 4.32 (2H, q, J= 7.3) Hz, 8.19 (IH, s>

Reference： [1]Patent: WO2007/8140,2007,A1 .Location in patent: Page/Page column 194

20
[ 3424-43-9 ]
[ 1174665-76-9 ]

Yield	Reaction Conditions	Operation in experiment
92%	With N-iodo-succinimide; In acetonitrile; at 95℃; for 5.0h;	N-lodosuccinimide (4Og, 180mmol) was added to a suspension of intermediate (5b), 2-methyl-6-oxo-1 ,6-dihydro-pyridine-3-carboxylic acid ethyl ester (18.1g, lOOmmol) in acetonitrile (40OmL), under a nitrogen atmosphere. The resulting suspension was heated at 950C for 5 hours to give an initial orange solution. An off-white precipitate slowly formed. The resulting suspension was allowed to cool and was poured into water (120OmL) to give an off-white precipitate. The separated by filtration and the <n="51"/>solids washed with water (50OmL) to give an off-white powder. The solids were dried in vacuo (6O0C) to give the product as an off-white powder, 28.3g (92%)

Reference： [1]Patent: WO2009/93012,2009,A1 .Location in patent: Page/Page column 23; 49-50

21
[ 53256-26-1 ]
[ 3424-43-9 ]

Yield	Reaction Conditions	Operation in experiment
36%	In N,N-dimethyl-formamide; at 175℃; for 24.0h;	A solution of intermediate (5a), (E)-4-[1-amino-eth-(Z)-ylidene]-pent-2-enedioic acid diethyl ester (51 g, 225mmol) in N,N-dimethylformamide (25OmL) was heated at 1750C for 24 hours to give a dark brown solution. The resulting solution was allowed to cool and a pale brown precipitate slowly formed. The precipitate was removed by filtration and the solids washed with dichloromethane (75ml_) and hexane (10OmL) to give a pale yellow powder. The solids were dried in vacuo (6O0C) to give the title compound as a pale yellow powder, 14.45g (36%)

Reference： [1]Patent: WO2009/93012,2009,A1 .Location in patent: Page/Page column 23; 49

22
[ 53256-25-0 ]
[ 3424-43-9 ]

Yield	Reaction Conditions	Operation in experiment
60%	In N,N-dimethyl-formamide; at 165℃; for 14.0h;	Step B ethyl 2-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate 5-Ethyl 1-methyl (2E,4Z)-4-(1-aminoethylidene)pent-2-enedioate (10 g, 50 mmol) and DMF (30 mL) were mixed in one 100 mL flask, and the mixture was stirred at 165 C. for 14 hrs. The reaction mixture was cooled to room temperature, then filtered to give the crude product, which was washed with DMF and small amount of methanol to give 5 g (60% yield) of the pure product. LC-MS found: 182.1 (M+H)+.

Reference： [1]Patent: US2013/96144,2013,A1 .Location in patent: Paragraph 0434; 0435
[2]Journal of Medicinal Chemistry,2010,vol. 53,p. 3814 - 3830
[3]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

23
[ 3424-43-9 ]
[ 1315544-62-7 ]

Reference： [1]Patent: WO2011/87776,2011,A1
[2]Journal of Medicinal Chemistry,2018,vol. 61,p. 5245 - 5256

24
[ 3424-43-9 ]
[ 1315544-63-8 ]

Reference： [1]Patent: WO2011/87776,2011,A1
[2]Journal of Medicinal Chemistry,2018,vol. 61,p. 5245 - 5256

25
[ 141-97-9 ]
[ 3424-43-9 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552
[2]Bioorganic and Medicinal Chemistry Letters,2018,vol. 28,p. 922 - 925

26
[ 3424-43-9 ]
2-hydroxy-6,7-dihydro-5H-cyclopenta[b]pyridin-5-one [ No CAS ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

27
[ 3424-43-9 ]
[ 1359669-60-5 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

28
[ 3424-43-9 ]
C₂₃H₂₂ClNO₄S [ No CAS ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

29
[ 3424-43-9 ]
[ 1359669-62-7 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

30
[ 3424-43-9 ]
[ 1359668-78-2 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

31
[ 3424-43-9 ]
[ 1359668-80-6 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

32
[ 3424-43-9 ]
[ 41598-57-6 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

33
[ 3424-43-9 ]
[ 31163-14-1 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552

34
[ 3424-43-9 ]
[ 31163-13-0 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552
[2]Patent: WO2018/140809,2018,A1

35
[ 626-34-6 ]
[ 3424-43-9 ]

Reference： [1]Journal of Medicinal Chemistry,2012,vol. 55,p. 1538 - 1552
[2]Patent: US2013/96144,2013,A1

36
[ 3424-43-9 ]
[ 1196145-86-4 ]

Yield	Reaction Conditions	Operation in experiment
93%	With phosphorus(V) oxybromide; at 130℃; for 4.0h;	Step C ethyl 6-bromo-2-methylnicotinate Ethyl 2-methyl-6-oxo-1,6-dihydropyridine-3-carboxylate (2.0 g, 11 mmol) and POBr3 (8.9 g, 31 mmol) were mixed in one 100 mL flask, and the mixture was stirred at 130 C. for 4 hrs. The reaction mixture was cooled to room temperature and 50 g of ice water was added. The mixture was neutralized to pH=9 with aqueous NaHCO3 solution, extracted twice with EtOAc, dried over sodium sulfate, filtered and concentrated under reduced pressure to give 2.5 g (93% yield) of the desired product. LC-MS found: 244.1 (M+H)+.

Reference： [1]Patent: US2013/96144,2013,A1 .Location in patent: Paragraph 0436; 0437

37
[ 3424-43-9 ]
[ 1430058-73-3 ]