L-Aspartic acid diethyl ester hydrochloride → 1,4-Dimethyl L-aspartate

HRID 1885417노트

반응식

HRID 1885417 반응식
Cl.[CH2:2]([O:4][C:5](=[O:14])[C@H:6]([CH2:8][C:9]([O:11][CH2:12]C)=[O:10])[NH2:7])C>C(=O)([O-])[O-].[Na+].[Na+]>[NH2:7][C@H:6]([C:5]([O:4][CH3:2])=[O:14])[CH2:8][C:9]([O:11][CH3:12])=[O:10]

참가 물질

3

반응물 1

HCID 12416466L-Aspartic acid diethyl ester hydrochloride

생성물 1

HCID 1112071,4-Dimethyl L-aspartate수율 84.3%

시약·촉매·용매 1

HCID 10340Sodium Carbonate용매

실험 절차

Diethylaspartate hydrochloride (3, 85.31 g, 0.432 mol) was dissolved in a saturated solution of aqueous sodium carbonate (200 mL) and extracted with ethyl acetate (10×250 mL) in a separatory funnel. The combined organic phases were dried by filtration through magnesium sulfate and sodium sulfate and concentrated in vacuo to provide dimethyl aspartate (58.73 g, 0.364 mol, 84%) as a pale yellow oil. This material provided satisfactory 1H NMR data and was used immediately in the preparation of N-benzyloxycarbonylglycyl-L-α-aspartic acid dimethyl ester (5).

후처리

  1. extractionextracted with ethyl acetate (10×250 mL) in a separatory funnel
  2. dry with materialThe combined organic phases were dried by filtration through magnesium sulfate and sodium sulfate
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a0f6b6fcd7e244e89c1dbf6460731807
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05144073

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