Monobenzone → 1-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine

HRID 894970노트

반응식

HRID 894970 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:21][CH2:20]1>CS(C)=O.[OH-].[Na+]>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:17][CH2:18][N:19]2[CH2:24][CH2:23][N:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:21][CH2:20]2)=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 7638MonobenzoneHCID 47418781-(2-Chloroethyl)-4-phenylpiperazine

생성물 1

HCID 129411031-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 14798Sodium Hydroxide용매2회

실험 절차

26.25 ml 4 N NaOH (.105 mol) was added to a stirred mixture of 21.0 g (0.105 mol) 4-benzyloxyphenol and 22.5 g (0.1 mol) of 1-(2-chloroethyl)-4-phenylpiperazine in 250 ml DMSO and the reaction was heated at 60° for 60 min. After cooling, the stirred mixture was diluted with 50 ml 1 N NaOH solution and the resulting crystalline precipitate was collected by filtration and washed with water to give, after drying in vacuo, essentially pure end product, mp 116°-119°.

후처리

  1. temperaturethe reaction was heated at 60° for 60 min
  2. temperatureAfter cooling
  3. filtrationthe resulting crystalline precipitate was collected by filtration
  4. washwashed with water
  5. customto give
  6. customafter drying in vacuo, essentially pure end product, mp 116°-119°

출처 및 근거

ORD 기록
ord-b470df3689434c34bdd3071a8273085e
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04285873

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