Sodium Hydroxide → ethyl (R)-2-acetylamino-3-(3,4-diethyl-phenyl)-propionate

HRID 644312노트

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HRID 644312 반응식
O.O.P([O-])([O-])(O)=O.[Na+].[Na+].O.O.P([O-])(O)(O)=O.[Na+].[C:18]([NH:21][CH:22]([CH2:28][C:29]1[CH:34]=[CH:33][C:32]([CH2:35][CH3:36])=[C:31]([CH2:37][CH3:38])[CH:30]=1)[C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:20])[CH3:19].[OH-].[Na+]>O.CC(C)=O>[C:18]([NH:21][C@H:22]([CH2:28][C:29]1[CH:34]=[CH:33][C:32]([CH2:35][CH3:36])=[C:31]([CH2:37][CH3:38])[CH:30]=1)[C:23]([O:25][CH2:26][CH3:27])=[O:24])(=[O:20])[CH3:19]

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 6451167Sodium Phosphate, Dibasic, DihydrateHCID 23673460Sodium Phosphate, Monobasic, DihydrateHCID 68580167Ethyl 2-acetylamino-3-(3,4-diethyl-phenyl)-propionate

생성물 1

HCID 69711472ethyl (R)-2-acetylamino-3-(3,4-diethyl-phenyl)-propionate

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

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온도
37 °C

실험 절차

27 mL Alcalase 2.4 L FG (Novozymes A/S; DK 2880 Bagsvaerd) were added to a solution of 38.0 g (213.5 mmol) disodium hydrogen phosphate dihydrate in 500 mL water at a temperature of 37° C. and the pH was adjusted to 7.5 by the addition of sodium dihydrogen phosphate dihydrate. Then at 37° C. with stirring 29.7 g (101.9 mmol) ethyl 2-acetylamino-3-(3,4-diethyl-phenyl)-propionate dissolved in 150 mL acetone was added dropwise. The pH value of the reaction mixture was kept constantly kept in the range from pH 7.4 to pH 7.6 by the addition of 1 M NaOH. After the addition had ended the mixture was stirred for 4 h at 37° C. The reaction mixture was extracted three times with tert-butylmethylether, the combined organic extracts were washed with 15% K2CO3 solution, dried and evaporated down under reduced pressure.

후처리

  1. additionwas added dropwise
  2. additionAfter the addition
  3. extractionThe reaction mixture was extracted three times with tert-butylmethylether
  4. washthe combined organic extracts were washed with 15% K2CO3 solution
  5. customdried
  6. customevaporated down under reduced pressure

출처 및 근거

ORD 기록
ord-99511db54e5c49239f9ad7e1ff2476cf
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700589B2

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