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1-[4,4-Bis(4-fluorophenyl)butyl]-4-(phenylmethyl)-2-piperazinecarboxamide → 1-[4,4-Bis(4-fluorophenyl)butyl]-2-piperazinecarboxamide

HRID 35319
ノート
印刷プレビュー

反応式

HRID 35319 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:28]2[CH:33]=[CH:32][C:31]([F:34])=[CH:30][CH:29]=2)[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][N:15](CC3C=CC=CC=3)[CH2:14][CH:13]2[C:25]([NH2:27])=[O:26])=[CH:4][CH:3]=1.[H][H]>[Pd].CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:28]2[CH:29]=[CH:30][C:31]([F:34])=[CH:32][CH:33]=2)[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH:13]2[C:25]([NH2:27])=[O:26])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 212956801-[4,4-Bis(4-fluorophenyl)butyl]-4-(phenylmethyl)-2-piperazinecarboxamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 138832881-[4,4-Bis(4-fluorophenyl)butyl]-2-piperazinecarboxamide収率 66.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 14.8 parts of 1-[4,4-bis(4-fluorophenyl)butyl]-4-(phenylmethyl)-2-piperazinecarboxamide and 200 parts of methanol was hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen was taken up, the catalyst was filtered off and the filtrate was evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (85:15 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 2,2'-oxybispropane, yielding 7.9 parts (66.4%) of 1-[4,4-bis(4-fluorophenyl)butyl]-2-piperazinecarboxamide; m.p. 113.6° C. (intermediate 53).

後処理

  1. filtrationthe catalyst was filtered off
  2. customthe filtrate was evaporated
  3. customThe residue was purified by column-chromatography over silica gel using
  4. additiona mixture of trichloromethane and methanol (85:15 by volume) as eluent
  5. customThe pure fractions were collected
  6. customthe eluent was evaporated
  7. customThe residue was crystallized from 2,2'-oxybispropane

出典と根拠

ORDレコード
ord-87164c71da6b490c94839b1f49e4f1fe
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04766125

反応ノート

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