Triethylamine → 1-(4-Benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone

HRID 370657

반응식

HRID 370657 반응식
[C:1]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[CH2:27]([O:34][C:35]1[CH:40]=[CH:39][C:38]([C:41](=[O:44])[CH2:42]Br)=[CH:37][CH:36]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>C(OCC)(=O)C>[CH2:27]([O:34][C:35]1[CH:36]=[CH:37][C:38]([C:41](=[O:44])[CH2:42][N:11]2[CH2:10][CH2:9][N:8]([CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:13][CH2:12]2)=[CH:39][CH:40]=1)[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 70048BenzhydrylpiperazineHCID 105425931-[4-(Benzyloxy)phenyl]-2-bromoethan-1-one

생성물 1

HCID 103227601-(4-Benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone수율 87.4%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To 90 ml of an ethyl acetate solution containing 7.56 g (30 mmol) of 1-diphenylmethylpiperazine and 3.33 g (33 mmol) of triethylamine was added 9.15 g (30 mmol) of p-benzyloxy-α-bromoacetophenone. The resultant mixture was stirred at room temperature for 45 minutes. After addition of 100 ml of ice water, the thus obtained mixture was stirred for about 10 minutes. Precipitated crystals were collected by filtration and then washed successively with water, ethanol and ethyl acetate and thereafter dried to give 12.5 g of 1-(4-benzyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanone (yield: 87.4%).

후처리

  1. customPrecipitated crystals
  2. filtrationwere collected by filtration
  3. washwashed successively with water, ethanol and ethyl acetate
  4. customdried

출처 및 근거

ORD 기록
ord-646b829131ad47e7ae5bb7ff444ff8bf
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528194

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