Hydrogen chloride-ethyl acetate → (2S,3R)-2-amino-3-methoxy-N,N-dimethyl-butanamide

HRID 1620712노트

반응식

HRID 1620712 반응식
C(OC([NH:8][C@H:9]([C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[C@@H:10]([CH3:13])[O:11][CH3:12])=O)(C)(C)C.Cl.C(OCC)(=O)C>C(OCC)(=O)C>[CH3:18][N:16]([CH3:17])[C:14](=[O:15])[C@H:9]([C@@H:10]([CH3:13])[O:11][CH3:12])[NH2:8]

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86678875N2-(tert-butoxycarbonyl)-N,N,O-trimethyl-L-threoninamide

생성물 1

HCID 86678876(2S,3R)-2-amino-3-methoxy-N,N-dimethyl-butanamide수율 96.5%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of N2-(tert-butoxycarbonyl)-N,N,O-trimethyl-L-threoninamide (2.02 g) in ethyl acetate (10 mL) was added 4N hydrogen chloride/ethyl acetate solution (10 mL) at room temperature. The reaction mixture was stirred at room temperature for 3 hr, and the reaction mixture was concentrated under reduced pressure. To the reaction mixture was added methanol (10 mL). To the reaction mixture was added AMBERLYST (registered trademark) A21 (1.00 g) at room temperature. The reaction mixture was stirred at room temperature for 1 hr, the insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure to give the title compound (1.20 g).

후처리

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionTo the reaction mixture was added methanol (10 mL)
  3. additionTo the reaction mixture was added AMBERLYST (registered trademark) A21 (1.00 g) at room temperature
  4. stirringThe reaction mixture was stirred at room temperature for 1 hr
  5. customthe insoluble material was removed by filtration
  6. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-21aebf40720245edb09ad6e3babbb3fc
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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