Ammonia → HCID 68620036, 화합물

HRID 1725568노트

반응식

HRID 1725568 반응식
[CH3:1][CH:2]([C:14](=O)[CH3:15])[C:3]([NH:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)=[O:4].[NH3:17].[Cl-].[Al+3].[Cl-].[Cl-]>C(OCC)C>[CH2:6]([NH:5][C:3](=[O:4])[C:2]([CH3:1])=[C:14]([NH2:17])[CH3:15])[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 6451240Aluminum(III) ChlorideHCID 119843462-methyl-3-oxo-N-phenethyl-butyramide

생성물 1

HCID 68620036HCID 68620036, 화합물수율 85%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A solution of 2-methyl-3-oxo-N-phenethyl-butyramide of Example 1d (1.10 g, 5.00 mmol) in diethyl ether (300 mL) was saturated with gaseous ammonia for 3 h while cooled in an ice bath. Anhydrous aluminum chloride (99.99% purity, 0.667 g, 5.00 mmol) was then added in small portions and the reaction was allowed to stir at room temperature overnight. The reaction mixture was filtered and concentrated under reduced pressure to give 3-amino-2-methyl-but-2-enoic acid phenethyl-amide (0.97 g, 85% conversion by NMR) as a white solid which was used without purification for the next synthetic step.

후처리

  1. temperaturewhile cooled in an ice bath
  2. filtrationThe reaction mixture was filtered
  3. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a1aac1e4bce847a19f7a67e3232eeced
출처 데이터셋
uspto-grants-2009_02
특허 번호
US07491728B2

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