Ammonium Chloride → HCID 20309064、化合物

HRID 1438815ノート

反応式

HRID 1438815 の反応式
[CH2:1]([N:8]([CH2:10][C:11](=[O:25])[CH:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH3:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:26][Mg]I.[Cl-].[NH4+]>CCOCC>[CH2:1]([N:8]([CH2:10][C:11]([CH3:26])([OH:25])[CH:12]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1)[CH3:9])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 125490473-[Benzyl(methyl)amino]-1,1-diphenylpropan-2-oneHCID 178418373HCID 178418373、化合物

生成物 1

HCID 20309064HCID 20309064、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

実験手順

3-(N-Benzyl N-methylamino)-1,1-diphenyl-propan-2-one (10g) in dry ether (250 ml.) was added to a solution of methyl magnesium iodide (from 2.4g. magnesium and 14.2g methyl iodide) in dry ether (250 ml.) and the mixture heated at reflux for 2 hours. Saturated ammonium chloride solution was added; isolation through ether in the usual manner gave 3-(N-benzyl,N-methylamino)-2-methyl-1,1-diphenyl-propan-2-ol, purified by chromatography on alumina using progressively graded mixtures of light petroleum and ether as eluant and isolated as the hyrochloride (6.8g., 65%, m.p. 121° - 124° (from ethanol-ether).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 2 hours

出典と根拠

ORDレコード
ord-2bccd52e3e8c46f88159378d66949fad
出典データセット
uspto-grants-1977_11
特許番号
US04056630

反応ノート

読み込み中…