Benzhydryl 2-chloroethyl ether → 2-(diphenylmethoxy)ethyl-N-methyl-N'-methylpropanediamine

HRID 129729ノート

反応式

HRID 129729 の反応式
[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[O:8][CH2:9][CH2:10]Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:18][NH:19][CH:20]([NH:23][CH3:24])[CH2:21][CH3:22]>C1(C)C=CC=CC=1>[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[O:8][CH2:9][CH2:10][C:20]([NH:23][CH3:24])([NH:19][CH3:18])[CH2:21][CH3:22])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 141724Benzhydryl 2-chloroethyl etherHCID 22287041HCID 22287041、化合物

生成物 1

HCID 217598692-(diphenylmethoxy)ethyl-N-methyl-N'-methylpropanediamine収率 63%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 3 g (12.2 mmole) of 2- (diphenyl-methoxy)ethyl chloride, 5 g (49 mmole) of N,N' -dimethyl-propanediamine and 40 ml of toluene was heated under reflux overnight. At the end of this time, the toluene layer was separated and washed with water; 25 ml of a 10% w/v aqueous solution of acetic acid was then added thereto. The aqueous layer was separated, and a 10% w/v aqueous solution of sodium hydroxide was added to make it alkaline. The mixture was then extracted with diethyl ether, and the solvent was removed by distillation under reuced pressure, to obtain 2.4 g (yield 63%) of the title compound as an oil.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. customAt the end of this time, the toluene layer was separated
  4. washwashed with water
  5. addition25 ml of a 10% w/v aqueous solution of acetic acid was then added
  6. customThe aqueous layer was separated
  7. additiona 10% w/v aqueous solution of sodium hydroxide was added
  8. extractionThe mixture was then extracted with diethyl ether
  9. customthe solvent was removed by distillation under reuced pressure

出典と根拠

ORDレコード
ord-02b3f8aa00f246cba28b781a2959ff3d
出典データセット
uspto-grants-1995_11
特許番号
US05470851

反応ノート

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