Acetic Anhydride → N-acetyl-N-methyl-L-alanine methyl ester

HRID 1660103노트

반응식

HRID 1660103 반응식
Cl.[CH3:2][O:3][C:4](=[O:9])[C@H:5]([CH3:8])[NH:6][CH3:7].[C:10](OC(=O)C)(=[O:12])[CH3:11].C(N(CC)CC)C.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.O>[CH3:2][O:3][C:4](=[O:9])[C@H:5]([CH3:8])[N:6]([C:10](=[O:12])[CH3:11])[CH3:7]

참가 물질

7

반응물 4

HCID 7918Acetic Anhydride2회HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 13850987N-Methyl-L-alanine methyl ester hydrochloride (1:1)

생성물 1

HCID 54357781N-acetyl-N-methyl-L-alanine methyl ester

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매2회

실험 절차

In 300 ml of chloroform was dissolved 33.7 g (0.22 mole) of N-methyl-L-alanine methyl ester.hydrochloride, followed by the addition of 65 ml of acetic anhydride and 110 ml of triethylamine. The mixture was allowed to stand at room temperature for 24 hours and, after the excess acetic anhydride was decomposed with water, was neutralized with sodium hydrogen carbonate. The chloroform layer was separated, the water layer was extracted with ethyl acetate (120 ml×5), and the chloroform and ethyl acetate layers were combined and concentrated under reduced pressure. The brown oil thus obtained was dissolved in chloroform, washed with aqueous sodium hydrogen carbonate and concentrated under reduced pressure. By the above procedure there was obtained 31.8 g of N-acetyl-N-methyl-L-alanine methyl ester as brown oil.

후처리

  1. customThe chloroform layer was separated
  2. extractionthe water layer was extracted with ethyl acetate (120 ml×5)
  3. concentrationconcentrated under reduced pressure
  4. customThe brown oil thus obtained
  5. washwashed with aqueous sodium hydrogen carbonate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-084927f84e3d41f3b12975bb5f3edf33
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04307016

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