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2-Vinylpyridine → (S)-5,11-Dihydro-5-[1-(2-[2-pyridyl]ethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine

HRID 1460479
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HRID 1460479 반응식
[CH:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)=[CH2:2].[NH:9]1[CH2:13][CH2:12][CH2:11][C@H:10]1[CH2:14][N:15]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[CH2:19][S:18][C:17]2[CH:26]=[CH:27][CH:28]=[CH:29][C:16]1=2>>[N:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[CH2:1][CH2:2][N:9]1[CH2:13][CH2:12][CH2:11][C@H:10]1[CH2:14][N:15]1[C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=2[CH2:19][S:18][C:17]2[CH:26]=[CH:27][CH:28]=[CH:29][C:16]1=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 75212-VinylpyridineHCID 22841647(S)-5,11-Dihydro-5-(2-pyrrolidinylmethyl)dibenzo[b,e][1,4]-thiazepine

생성물 1

HCID 53971647(S)-5,11-Dihydro-5-[1-(2-[2-pyridyl]ethyl)-2-pyrrolidinylmethyl]dibenzo[b,e][1,4]thiazepine수율 58.3%

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온도
120 °C

실험 절차

A mixture of 2-vinylpyridine (250 mg) and (S)-5,11-dihydro-5-(2-pyrrolidinylmethyl)dibenzo[b,e][1,4]thiazepine (see Preparations 13 and 14) (166 mg) was heated at 120° C. for 2 hours, cooled to room temperature and purified by chromatography on silica gel using ethyl acetate/methanol (10:1) as eluant. Appropriate fractions were combined and evaporated under reduced pressure to give the title compound as a pale brown gum, (131 mg, 58%).

후처리

  1. temperaturecooled to room temperature
  2. custompurified by chromatography on silica gel
  3. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-d590480b36894e7da85ba02f9b2180b9
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05071844

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