4-Benzhydrylpiperidine → HCID 12796197、化合物

HRID 127728

反応式

HRID 127728 の反応式
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

参加物

4

反応物 2

HCID 882784-BenzhydrylpiperidineHCID 12796194HCID 12796194、化合物

生成物 1

HCID 12796197HCID 12796197、化合物収率 149.6%

試薬・触媒・溶媒 1

HCID 6386tert-Butanol溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-555f25c28eb04998b04b819d870496e5
出典データセット
uspto-grants-1981_03
特許番号
US04256891

関連ノート

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