N-Methylbenzeneethanamine → N-methyl-N-phenethyl-2-bromoacetamide

HRID 129678

反応式

HRID 129678 の反応式
[Br:1][CH2:2][C:3](Cl)=[O:4].[CH3:6][NH:7][CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>C(Cl)Cl>[CH3:6][N:7]([CH2:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:3](=[O:4])[CH2:2][Br:1]

参加物

4

反応物 2

HCID 11503N-MethylbenzeneethanamineHCID 89602Bromoacetyl chloride

生成物 1

HCID 10753531N-methyl-N-phenethyl-2-bromoacetamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
-25 °C

実験手順

To a solution of 27.07 g (171.95 mmol) of bromoacetyl chloride in 100 ml of methylene chloride, cooled to -25° C. by means of an external cooling bath, is added dropwise a solution of 46.5 g (343.9 mmol) of N-methyl-N-phenethyl amine in 50 ml of methylene chloride over a period of 11/2 hours. The reaction mixture is stirred at -25° C. for additional 15 minutes and then allowed to equilibrate to room temperature. The reaction mixture is then partitioned between methylene chloride and water. The organic layer is washed with 1N aqueous HCl solution and water, dried over magnesium sulfate and concentrated in vacuo to give N-methyl-N-phenethyl-2-bromoacetamide which is used directly in the next step.

後処理

  1. customto equilibrate to room temperature
  2. customThe reaction mixture is then partitioned between methylene chloride and water
  3. washThe organic layer is washed with 1N aqueous HCl solution and water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-51a646d0e6b44ea480daff1cf989f545
出典データセット
uspto-grants-1995_11
特許番号
US05468898

関連ノート

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