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[ CAS No. 59-02-9 ]

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2D
Chemical Structure| 59-02-9
Chemical Structure| 59-02-9
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Product Details of [ 59-02-9 ]

CAS No. :59-02-9MDL No. :MFCD00072045
Formula :C29H50O2Boiling Point :485.9°C at 760 mmHg
Linear Structure Formula :OHC6(CH3)3OCH2CH2CCH3C16H33InChI Key :N/A
M.W :430.71Pubchem ID :-
Synonyms :

Computed Properties of [ 59-02-9 ]

TPSA : - H-Bond Acceptor Count : -
XLogP3 : - H-Bond Donor Count : -
SP3 : - Rotatable Bond Count : -

Safety of [ 59-02-9 ]

Signal Word:WarningClassN/A
Precautionary Statements:P261-P305+P351+P338UN#:N/A
Hazard Statements:H302-H315-H319-H335Packing Group:N/A
GHS Pictogram:

Application In Synthesis of [ 59-02-9 ]

  • Downstream synthetic route of [ 59-02-9 ]

[ 59-02-9 ] Synthesis Path-Downstream   1~10

  • 1
  • [ 108-30-5 ]
  • [ 59-02-9 ]
  • [ 4345-03-3 ]
YieldReaction ConditionsOperation in experiment
93.6% With sodium hydroxide; In butanone; at 40℃; for 6h; Low content of natural mixed tocopherol (vitamin E) 50 kg,Which mixed with tocopherol content of 38.2%, adding succinic anhydride 5.5 kg,10 kg of sodium hydroxide,Butanone 150 kg,Esterified at 40 degrees Celsius for 6 hours; after esterification, the ketone was removed by distillation under reduced pressure,Add 250 kg of cyclohexane to wash with water, add 100 kg of water each time,Washed three times to neutral, cooled to 15 degrees Celsius for 12 hours of crystallization; the crystalline solid separation,Dried to give natural tocopherol succinate.The content of natural tocopherol succinate was 93.6%.
85% dmap; triethylamine; In dichloromethane; at 25℃; According to the first method, ?-tocopherol or vitamin E (2.15 g, 5 mmol) and succinic anhydride (750 mg, 7.5 mmol, 1.5 eq) are dissolved in 20 ml of anhydrous dichloromethane (CH2Cl2). Dimethylaminopyridine (DMAP) (305 mg, 2.5 mmol, 0.5 eq) and anhydrous triethylamine (0.7 ml, 1 eq) are added thereto and the reaction is monitored by thin-layer chromatography (tlc) (Et2O/petroleum ether (PE) 2:3 or ethyl acetate/PE 1:1). The reaction is generally complete after reacting overnight, and the mixture is thus filtered and then washed with aqueous 5% hydrochloric acid (HCl). The organic phase is dried over MgSO4 and then evaporated to give a yellow oil (about 3 g) to be purified.In both cases, the product is purified by flash chromatography (2.5 cm?16 cm column, eluent Et2O/PE 2:3, 10-15 ml fractions). The deposition of the pasty oil may take place as a solid deposit or in CH2Cl2. The first method gives 2.26 g of pure CV-104.Rf (Et2O/PE 2:3): 0.39. 1H NMR (CDCl3, 250 MHz):2.87 (dt, 4H, H(Cac succ) 2J=21, 3J=6.6); 2.58 (t, 4H, H(C4, C3), 3J=6); 2.08, 2.01, 1.97 (3 s, 9H, CH3(C5), CH3(C7), CH3(C8)), 1.6-1 (broad multiplet, 24H, CH3(C1)+9?CH2, 3?CH tocopherol), 0.88, 0.84 (2 s, 12H, 4?CH3 tocopherol). 13C NMR (CDCl3, 50 MHz): 177.51, 170.96 (s, C=Oacid+C=Oester); 149.48 (s, C8a); 140.44 (s, C6); 126.73 (s, C7); 125.00 (s, C5); 123.10 (s, C8); 117.45 (s, C4a); 75.11 (s, C2) ; 39.42 (t, C1?); 37.45 (t, C7?+C9?+C3?+C5?+C11?); 32.83 (d, C8?+C4?+C12?); 28.97, 28.68, 24.88, 24.50, 21.08, 20.64 (C10?+C66?+C2?+C4+CH2 ac succ); 28.04 (CH3(C2)); 22.69 (C13?); 19.74, 12.7, 12.18, 12.10, 11.99 (CH(C12?+C8?+C4?)+CH3(C8+C7+C5)+CH3(C1)). IR (NaCl): 2924, 2856, 2735, 2638, 2540, 1746, 1694, 1455, 1421, 1378, 1323, 1246, 1155, 1106, 919, 853, 799, 728. MS (CI, NH3): 548 ([MNH4]+, 100); 531 ([MH]+, 11.3); 530 ([M]+, 3.4). UV (CH3CN): 286 (0.047 at a concentration of 14 ?g/ml); 203 (0.61 at a concentration of 14 ?g/ml). EA for C33H54O5 (530.78): calc. C, 74.67; H, 10.25; exp. C, 74.85, H, 10
With triethylamine; In toluene; at 85℃; for 9h; General procedure: The method for the synthesis of alpha-T succinate, alpha-T3 succinate, gamma-T3 succinate and delta-T3 succinate was adapted from our previous work (Abu-Fayyad et al., 2015). The general reaction scheme is outlined in Fig. 1 A. The individual alpha-T, alpha-T3, gamma-T3 and delta-T3 isomers (1.2g) were first dissolved in 6mL toluene. Equimolar amounts of succinic anhydride were then mixed with the isomer solutions. The mixtures were then stirred at 85C in a paraffin oil bath. The temperature was maintained using an IKA RCT heater supported with an IKA ETS-D4 fuzzy digital thermometer (IKA works Inc., Wilmington, NC). The reaction was stopped after 9h and cooled to room temperature. Water was then added and the reaction mixture was extracted with dichloromethane. The upper oily layer was kept and the lower aqueous phase was further extracted with dichloromethane. The combined oily layers were then washed three times with 1N HCL (7mL each) and twice with water (8mL each). Following extraction, the collected oil layers was dried over anhydrous Na2SO4, filtered, and concentrated with a rotary evaporator. The concentrate was then mixed with Celite 545 for further purification on column chromatography. After backing the column with a silica gel slurry (230-400mesh size), the samples were eluted through the column with the aid of a gradient ethyl acetate/hexane solution with an increasing ethyl acetate fraction from 10% to 45%. After concentration, collected fractions afforded approximately 1g of each succinate derivative: alpha-T and alpha-T3 (white solids) and gamma-T3 and delta-T3 (yellow viscous liquids).
  • 2
  • (2R,3R,4S,5R,6R)-2-(acetoxymethyl)-6-((3-bromopyridin-2-yl)oxy)tetrahydro-2H-pyran-3,4,5-triyl triacetate [ No CAS ]
  • [ 59-02-9 ]
  • [ 129514-95-0 ]
YieldReaction ConditionsOperation in experiment
75.7% With boron trifluoride diethyl etherate; In dichloromethane; at 15℃; for 5h; Step 3: To a solution of (2R,3R,4S,5R,6R)-2-(acetoxymethyl)-6-((3-bromopyridin-2- yl)oxy)tetrahydro-2H-pyran-3,4,5-triyl triacetate (0.350 g) and a-tocopherol(0.598 g) in CH2CI2 (5 ml_) was added BF3.Et20 (47%, 0.629 g) at 15 C. The mixture was stirred for 5 hr at 15 C. The reaction mixture was quenched with sodium bicarbonate solution (5 ml_), and extracted three times with dichloromethane (10 ml_). The combined organic layers were washed with brine (10 ml_), dried over Na2SC>4, filtered and concentrated under reduced pressure. The residue was purified by prep-TLC (S1O2, petroleum ether / Ethyl acetate, 5:1 ) to give [(2R,3R,4S,5R,6S)-3,4,5-triacetoxy-6-[(2R)-2,5,7,8-tetramethyl-2-[(4R,8R)- 4,8,12-trimethyltridecyl]chroman-6-yl]oxy-tetrahydropyran-2-yl]methyl acetate (0.400 g, 75.7% yield) as a white solid. NMR (400 MHz, CDC ): d 5.362 - 5.179 (m, 3H), 4.724 (d, 1 H), 4.191 - 4.049 (m, 3H), 3.536 (m, 1 H), 2.568 (m, 2H), 2.152 (s, 3H), 2.120 (s, 3H), 2.1 05 (s, 3H), 2.082 (s, 3H), 2.054 - 2.027 (m, 9H), 1 .838 - 1 .737 (m, 2H), 1 .572 - 1 .042 (m, 24H), 0.882 - 0.842 (m, 12H) ppm
75.7% With boron trifluoride diethyl etherate; In dichloromethane; at 15℃; for 5h; To a solution of [(1 R,2R,3S,4S,5S)-2,3,4-triacetoxy-5-[(3-bromo-2- pyridyl)oxy]cyclohexyl]methyl acetate (0.350 g) and a-tocopherol (0.598 g) in DCM (5 mL) was added BF3.Et20 (47%, 0.629 g,3 eq) at 15 C. The mixture was stirred for 5 hr at 15 C. The reaction mixture was quenched with sodium bicarbonate solution (5 mL), and extracted three times with dichloromethane (10 mL). The combined organic layers were washed with brine (10 mL), dried over Na2SC>4, filtered and concentrated under reduced pressure. The residue was purified by prep-TLC (S O , petroleum ether / Ethyl acetate, 5:1 ) to give [(2R,3R,4S,5R,6S)-3,4,5-triacetoxy-6-[(2R)-2,5,7,8-tetramethyl-2-[(4R,8R)- 4,8,12-trimethyltridecyl]chroman-6-yl]oxy-tetrahydropyran-2-yl]methyl acetate (0.400 g, 75.7% yield) as a white solid. 1H NMR (400 MHz, CDCI3) 5.362 - 5.179 (m,3H),4.724 (d,1 H),4.191 - 4.049 (m,3H),3.536 (m,1 H), 2.568 (m, 2H), 2.152 (s,3H), 2.120 (s,3H), 2.105 (s,3H), 2.082 (s,3H), 2.054 - 2.027 (m,9H),1 .838 - 1 .737 (m, 2H),1 .572 - 1 .042 (m, 24H), 0.882 - 0.842 (m,12H)
  • 3
  • [ 22118-09-8 ]
  • [ 59-02-9 ]
  • (R)-2,5,7,8-tetramethyl-2-((4R,8R)-4,8,12-trimethyltridecyl)chroman-6-yl 2-bromoacetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
92% A dry 300 mL two-necked round flask was filled with Ar gas, and then After taking the alpha- tocopherol 50 g (0.116 mol) dissolved in 100 mL of chloroform, and then 15 g (0.148 mol) of triethylamine (TEA) was added slowly in an ice bath. The mixture was stirred at low temperature for 30 minutes, and 20 g (0.127 mol) of bromoacetyl chloride was taken and droppedwise using a dropping funnel for 20 minutes. The addition continued at low temperature. After the addition was completed, the mixture was stirred for about 20 minutes while maintaining the low temperature, and the mixture was allowed to react for 3 hours in a shade state at room temperature. After completion of the reaction, and then the solution was transferred to a separating funnel with 100 mL of chloroform, and then washed with a diluted hydrochloric acid solution and distilled water, and the organic layer was separated and sufficiently dehumidified with MgSO4. After the desiccant was removed, the filtrate was concentrated under reduced pressure to obtain 58.9 g (yield: 92%) of alpha -Tocopheryl bromoacetate as a dark brown syrup.
  • 4
  • [ 70475-59-1 ]
  • [ 59-02-9 ]
  • 5-(((2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)chroman-6-yl)oxy)carbonyl)benzene-1,2,3-trityl triacetate [ No CAS ]
YieldReaction ConditionsOperation in experiment
85% With triethylamine; In dichloromethane; at 5 - 20℃; for 5h; Alpha-tocopherol (1.87 g), dichloromethane (10 ml) and triethylamine (0.8 ml) are placed in a 100 ml flask and stirred at low temperature (5 degrees).To this is added dropwise a solution of 3,4,5-triacetoxybenzoyl chloride obtained in the previous reaction in dichloromethane (10 ml).The mixture was stirred at room temperature for 5 hours and the reaction solution was concentrated under reduced pressure. The concentrated solution was dissolved in ethyl acetate (50 ml), washed with water,It is washed with a saturated sodium bicarbonate aqueous solution and saturated brine. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure and then separated by column chromatography to obtain 2.63 g (85%) of a yellow liquid.
  • 5
  • [ 39657-47-1 ]
  • [ 59-02-9 ]
  • 2,5,7,8-tetramethyl-2-(4,8,12-trimethyltridecyl)chroman-6-yl 4-acetonyl-3,5-dimethoxybenzoate [ No CAS ]
YieldReaction ConditionsOperation in experiment
87% With triethylamine; In dichloromethane; at 5 - 20℃; for 5h; Alpha-tocopherol (1.87 g), dichloromethane (10 ml) and triethylamine (0.8 ml) are placed in a 100 ml flask and stirred at low temperature (5 degrees). A solution of 4-acetoxy-3,5-dimethoxybenzoyl chloride obtained in the previous reaction in dichloromethane (10 ml) is added dropwise thereto. The mixture was stirred at room temperature for 5 hours and the reaction solution was concentrated under reduced pressure. The concentrated solution was dissolved in ethyl acetate (50 ml), washed with water, a saturated aqueous solution of sodium hydrogencarbonate,Wash with saturated salt water. The organic layer was dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure and then separated by column chromatography to obtain 2.84 g (87%) of a yellow solid.
  • 6
  • [(1R,2R,3S,4S,5S)-2,3,4-triacetoxy-5-[(3-bromo-2-pyridyl)oxy]cyclohexyl]methyl acetate [ No CAS ]
  • [ 59-02-9 ]
  • [ 129514-95-0 ]
YieldReaction ConditionsOperation in experiment
75.7% With boron trifluoride diethyl etherate; In dichloromethane; at 15℃; for 5h; To a solution of [(1 R,2R,35,45,55)-2,3,4-triacetoxy-5-[(3-bromo-2- pyridyl)oxy]cyclohexyl]methyl acetate (0.350 g) and a-tocopherol(0.598 g) in 0H2012 (5 mL) was added BE3.Et20 (47%, 0.629 g, 3 eq) at 15 C. The mixture was stirred for 5 hr at 15 C. The reaction mixturewas quenched with sodium bicarbonate solution (5 mL), and extracted three times with dichloromethane(10 mL). The combined organic layers were washed with brine (1 0 mL), dried over Na2504, filtered andconcentrated under reduced pressure. The residue was purified by prep-TLC (5i02, petroleum ether /Ethyl acetate, 5:1) to give [(2R,3R,45,5R,65)-3,4,5-triacetoxy-6-[(2R)-2,5,7,8-tetramethyl-2-[(4R,8R)-4,8,1 2-trimethyltridecyl]chroman-6-yl]oxy-tetrahydropyran-2-yl]methyl acetate (0.400 g, 75.7% yield) as awhite solid. 1H NMR (400 MHz, 0D013): O 5.362 - 5.179 (m, 3H), 4.724 (d, 1 H), 4.191 - 4.049 (m, 3H),3.536 (m, 1H), 2.568 (m, 2H), 2.152 (s, 3H), 2.120 (s, 3H), 2.105 (s, 3H), 2.082 (s, 3H), 2.054-2.027(m,9H), 1.838 - 1.737 (m, 2H), 1.572 - 1.042 (m, 24H), 0.882 - 0.842 (m, 12H) ppm
  • 7
  • [ 59-02-9 ]
  • [ 572-09-8 ]
  • 3,4,6‑tri‑O‑acetyl‑1,2‑O‑(1‑tocopheroxyethylidene)‑α‑D-glucopyranose [ No CAS ]
YieldReaction ConditionsOperation in experiment
67% General procedure: To a solution of alpha-bromide 8alpha (1 mmol) and chloride 9alphaor 9beta (see Table 1, entries 11 and 12) in 4 cm3, anhydrousCH2Cl2was added TBAI (1 mmol) or TEABr (1 mmol)(see Table 1, entries 9 and 10) and 50 mg of MS 4A underan argon atmosphere at room temperature. The mixturewas stirred for 10 min, and a solution of phenol 1, 2, or3 (1 mmol) and DIPEA (1 mmol) in 2 cm3 of anhydrousCH2Cl2was added. The reaction mixture was refluxed for24 h, filtered through a Celite pad, and concentrated invacuo. The solid residue was redissolved in 10 cm3 CH2Cl2,washed with water and a solution of saturated NaHCO3,dried over anhydrous Na2SO4,and concentrated undervacuum. The crude product was purified by MPLC chromatographyand eluted with ethyl acetate-hexane to obtainorthoesters 10, 12, or 13. 3,4,6-Tri-O-acetyl-1,2-O-(1-tocopheroxyethylidene)-alpha-dglucopyranose(10, C43H68O11)Oil. 1H NMR (400 MHz,CDCl3):delta = 5.17 (d, 3J = 5.5 Hz, 1H, H-1?), 5.03-5.00 (m,1H, H-3?), 4.81 (dd, 3J = 2.4, 9.4 Hz, 1H, H-4?), 4.18-4.17(m, 2H, H-6?), 3.90-3.88 (m, 1H, H-5?), 3.66-3.60 (m,1H, H-2?), 2.57 (t, 3J = 6.6 Hz, 2H, H-4), 2.19, 2.16, 2.07(3xs, 9H, H-5a, 7a, 8b), 2.09, 2.05 (2xs, 9H, CH3CO),1.87 (s, 3H, H-8?), 1.80-1.78 (m, 2H, H-3), 1.40-1.21(m, 21H, H-1?-12?), 0.89-0.83 (m, 12H, H-4?a, 8?a, 12?a,13?) ppm; 13C NMR (100 MHz, CDCl3):delta = 170.6, 169.6,169.1 (CH3CO), 148.5 (C-8a), 141.9 (C-6), 130.0 (C-7),128.3 (C-8) 124.3 (C-7?), 123.0 (C-5), 117.8 (C-4a), 96.9(C-1?), 75.0 (C-2), 73.8 (C-2?), 70.4 (C-3?), 67.9 (C-4?),67.0 (C-5?), 63.1 (C-6?), 31.4 (C-3), 23.8 (C-8?), 22.7, 22.6(C-2a), 20.6 (C-4), 20.7 (CH3CO), 14.4, 13.6, 11.8 (C-5a,7a, 8b), and phytyl chain signals: 40.2, 39.3, 37.3-37.6,32.8, 32.7, 31.4, 27.9, 24.8, 24.4, 23.5, 23.3, 21.0, 19.7-19.6 ppm; IR (CHCl3) v= 2928, 2869, 1744, 1461, 1371,1232, 1087, 1040, 1002, 946, 907 cm-1; HRMS (ESI): calcdfor C43H68NaO11783.4659, found 783.4613.
  • 8
  • [ 59-02-9 ]
  • [ 4451-36-9 ]
  • 3,4,6‑tri‑O‑acetyl‑1,2‑O‑(1‑tocopheroxyethylidene)‑α‑D-glucopyranose [ No CAS ]
YieldReaction ConditionsOperation in experiment
65% General procedure: To a solution of alpha-bromide 8alpha (1 mmol) and chloride 9alphaor 9beta (see Table 1, entries 11 and 12) in 4 cm3, anhydrousCH2Cl2was added TBAI (1 mmol) or TEABr (1 mmol)(see Table 1, entries 9 and 10) and 50 mg of MS 4A underan argon atmosphere at room temperature. The mixturewas stirred for 10 min, and a solution of phenol 1, 2, or3 (1 mmol) and DIPEA (1 mmol) in 2 cm3 of anhydrousCH2Cl2was added. The reaction mixture was refluxed for24 h, filtered through a Celite pad, and concentrated invacuo. The solid residue was redissolved in 10 cm3 CH2Cl2,washed with water and a solution of saturated NaHCO3,dried over anhydrous Na2SO4,and concentrated undervacuum. The crude product was purified by MPLC chromatographyand eluted with ethyl acetate-hexane to obtainorthoesters 10, 12, or 13. 3,4,6-Tri-O-acetyl-1,2-O-(1-tocopheroxyethylidene)-alpha-dglucopyranose(10, C43H68O11)Oil. 1H NMR (400 MHz,CDCl3):delta = 5.17 (d, 3J = 5.5 Hz, 1H, H-1?), 5.03-5.00 (m,1H, H-3?), 4.81 (dd, 3J = 2.4, 9.4 Hz, 1H, H-4?), 4.18-4.17(m, 2H, H-6?), 3.90-3.88 (m, 1H, H-5?), 3.66-3.60 (m,1H, H-2?), 2.57 (t, 3J = 6.6 Hz, 2H, H-4), 2.19, 2.16, 2.07(3xs, 9H, H-5a, 7a, 8b), 2.09, 2.05 (2xs, 9H, CH3CO),1.87 (s, 3H, H-8?), 1.80-1.78 (m, 2H, H-3), 1.40-1.21(m, 21H, H-1?-12?), 0.89-0.83 (m, 12H, H-4?a, 8?a, 12?a,13?) ppm; 13C NMR (100 MHz, CDCl3):delta = 170.6, 169.6,169.1 (CH3CO), 148.5 (C-8a), 141.9 (C-6), 130.0 (C-7),128.3 (C-8) 124.3 (C-7?), 123.0 (C-5), 117.8 (C-4a), 96.9(C-1?), 75.0 (C-2), 73.8 (C-2?), 70.4 (C-3?), 67.9 (C-4?),67.0 (C-5?), 63.1 (C-6?), 31.4 (C-3), 23.8 (C-8?), 22.7, 22.6(C-2a), 20.6 (C-4), 20.7 (CH3CO), 14.4, 13.6, 11.8 (C-5a,7a, 8b), and phytyl chain signals: 40.2, 39.3, 37.3-37.6,32.8, 32.7, 31.4, 27.9, 24.8, 24.4, 23.5, 23.3, 21.0, 19.7-19.6 ppm; IR (CHCl3) v= 2928, 2869, 1744, 1461, 1371,1232, 1087, 1040, 1002, 946, 907 cm-1; HRMS (ESI): calcdfor C43H68NaO11783.4659, found 783.4613.
  • 9
  • [ 105-36-2 ]
  • [ 59-02-9 ]
  • [ 261929-52-6 ]
YieldReaction ConditionsOperation in experiment
88% With potassium hydroxide; In N,N-dimethyl-formamide; at 20℃; A solution of a-tocopherol (0.5 g, 1.16 mmol) in N,N-dimethylformamide(20 mL) was treated with ethyl bromo acetate(3.4 g, 8.3 mmol) and an excess of powdered KOH (1.2 g, 30 mmol).The resulting yellow residue was stirred vigorously for 24 h at room temperature. The reaction was acidified with 6 N HCl andextracted with ethyl acetate (3 30 mL). The combined ethyl acetate layers were washed with H2O (3 30 mL) and brine(1 30 mL), and then dried with Na2SO4. The ethyl acetate solutionwas concentrated to yellow oil and purified by silica gel chromatographyeluting with 20% (v/v) EtOAc and 1% acetic acid in hexanes. This yielded 1A as yellow color (0.50 g, 88%).1H NMR (400 MHz, CDCl3) d/ppm 0.8-0.90 (m, 12H), 1.00-1.50(m, 25H), 1.77-1.88 (m, 2H), 2.08 (s, 3H), 2.13 (s, 3H), 2.17 (s, 3H),2.55-2.50 (t, 2H), 4.3 (s, 2H), 7.98 (broad, 1H). ESI-MS: Calculated 488; found [M+18] 506.
  • 10
  • [ 79-41-4 ]
  • [ 59-02-9 ]
  • vitamin E methacrylate [ No CAS ]
YieldReaction ConditionsOperation in experiment
91% With dmap; In diethyl ether; at 50℃; Take 43.72 g of vitamin E (0.100 mol) and place in a 500 mL three-necked flask. ethyl ether was added thereto with stirring until the vitamin E was completely dissolved, and then 5 mg of DMAP (4-dimethylaminopyridine) was added thereto, followed by the addition of 13.23 g of a methacrylic acid (Compound 2, 0.16 mol) in a saturated diethyl ether solution. the mixture was slowly heated at 50 C under stirring to carry out the reaction, and use high performance liquid chromatography to track the reaction to the end point. Distilling diethyl ether under reduced pressure, and obtained solid is washed with water and freeze-dried, and then obtained off-white solid 45.39g (0.089mol), Melting point 42~43 C, yield is 91%.
91% With dmap; In diethyl ether; at 50℃; Preparation: Take 43.72 g of vitamin E (0.100 mol) and place in a 500 mL three-necked flask. diethyl ether was added thereto with stirring until the vitamin E was completely dissolved.Afterwards, 5 mg of DMAP (4-dimethylaminopyridine) was added thereto.Further, 13.23 g of a solution of methacrylic acid (Compound 2, 0.16 mol) in saturated diethyl ether was added.The reaction was slowly carried out while stirring to 50 C with stirring, and the reaction was traced to the end point by high performance liquid chromatography.The diethyl ether was distilled off under reduced pressure, and the obtained solid was washed with water and then dried.Obtained an off-white solid of 45.39 g (0.091 mol).Melting point 42 ~ 43 C,The yield was 91%.
91% With dmap; In diethyl ether; at 50℃; Preparation: Take 43.72 g of vitamin E (0.100 mol) and place in a 500 mL three-necked flask. diethyl ether was added thereto with stirring.Until the vitamin E is completely dissolved,Afterwards, 5 mg of DMAP (4-dimethylaminopyridine) was added thereto.Further, 13.23 g of a solution of methacrylic acid (Compound 2, 0.16 mol) in saturated diethyl ether was added.The reaction was slowly carried out while stirring to 50 C with stirring, and the reaction was traced to the end point by high performance liquid chromatography.The diethyl ether was distilled off under reduced pressure, and the obtained solid was washed with water and then dried.Obtained an off-white solid of 45.39 g (0.091 mol).Melting point 42 ~ 43 C,The yield was 91%.
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