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

HRID 1155411
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반응식

HRID 1155411 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 물질실험 절차후처리출처 및 근거반응 노트

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 (0.105 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-574fb20002cb4e42a14d9deeaa2ff1a0
출처 데이터셋
uspto-grants-1981_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04301300

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