4-Benzhydrylpiperidine → HCID 12796197, 화합물

HRID 127728

반응식

HRID 127728 반응식
C1(C)C=CC(S(O[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[C:22](=[O:23])[CH2:21][O:20][CH2:19][C:18]2=[O:24])(=O)=O)=CC=1.[CH:26]([CH:39]1[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]1)([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C(O)(C)(C)C>[CH:26]([CH:39]1[CH2:44][CH2:43][N:42]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][N:17]2[C:18](=[O:24])[CH2:19][O:20][CH2:21][C:22]2=[O:23])[CH2:41][CH2:40]1)([C:33]1[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1)[C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1

참가 물질

4

반응물 2

HCID 882784-BenzhydrylpiperidineHCID 12796194HCID 12796194, 화합물

생성물 1

HCID 12796197HCID 12796197, 화합물수율 149.6%

시약·촉매·용매 1

HCID 6386tert-Butanol용매2회

실험 절차

To a solution of 9.75 grams (26.39 millimoles) of 6-(3,5-dioxomorpholino)hexyl p-toluenesulfonate (prepared as described in Example IX) in 160 milliliters of warm tertiary butyl alcohol was added portionwise at temperatures in the range of 30°-32° C. over a period of about 23 minutes, 63 grams (26.38 millimoles) of 4-benzhydrylpiperidine in 160 milliliters of tertiary-butyl alcohol. The reaction mixture was heated at reflux temperature for about 22 hours and thereafter the solvent removed by vaporization to obtain 17.7 grams of a 4-[6-(4-benzhydrylpiperidino)hexyl]-3,5-dioxomorpholine product as a yellow oil. Crystallization (twice) from ethyl acetate produced 4.19 grams of white crystals, m.p., 121°-124.5° C. and having NMR, UV and IR spectral characteristics appropriate for the product.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux temperature for about 22 hours
  3. customthe solvent removed by vaporization

출처 및 근거

ORD 기록
ord-555f25c28eb04998b04b819d870496e5
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04256891

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