Ammonia → HCID 68620036、化合物

HRID 1725568ノート

反応式

HRID 1725568 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 68620036HCID 68620036、化合物収率 85%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-a1aac1e4bce847a19f7a67e3232eeced
出典データセット
uspto-grants-2009_02
特許番号
US07491728B2

反応ノート

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