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

HRID 129729노트

반응식

HRID 129729 반응식
[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

참가 물질

4

반응물 2

HCID 141724Benzhydryl 2-chloroethyl etherHCID 22287041HCID 22287041, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-02b3f8aa00f246cba28b781a2959ff3d
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05470851

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