HCID 18187860、化合物 → HCID 18187489、化合物

HRID 1357910ノート

反応式

HRID 1357910 の反応式
C(OC([N:11]1[CH2:16][CH2:15][CH:14]([CH2:17][CH2:18][C:19]([F:27])([F:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:13][CH2:12]1)=O)C1C=CC=CC=1>C(O)C.[OH-].[OH-].[Pd+2]>[F:27][C:19]([F:26])([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH2:18][CH2:17][CH:14]1[CH2:13][CH2:12][NH:11][CH2:16][CH2:15]1

参加物

4

反応物 1

HCID 18187860HCID 18187860、化合物

生成物 1

HCID 18187489HCID 18187489、化合物収率 103.6%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒2 回HCID 702Ethanol溶媒

実験手順

The partially purified 1-(benzyloxycarbonyl)-4-(3,3-difluoro-3-phenylprop-1-yl)piperidine (247 mg) was hydrogenated at atmospheric pressure in 95% ethanol (4.0 mL) containing 20% Pd(OH)2/C (60 mg). After 6 h, additional 20% Pd(OH)2/C (32 mg) was added and the hydrogenation was continued for another 16 h. The mixture was filtered and the catalyst was washed with 95% ethanol. Evaporation of the filtrate gave 164 mg of crude 4-(3,3-difluoro-3-phenylprop-1-yl)piperidine as a colorless syrup.

後処理

  1. waitthe hydrogenation was continued for another 16 h
  2. filtrationThe mixture was filtered
  3. washthe catalyst was washed with 95% ethanol
  4. customEvaporation of the filtrate

出典と根拠

ORDレコード
ord-0d37063047fe48289d6feb67f1c5338f
出典データセット
uspto-grants-2003_07
特許番号
US06593346B2

反応ノート

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