Methanol → Benzenamine, 4-(4-(4-methoxyphenyl)-1-piperazinyl)-

HRID 1164218

反応式

HRID 1164218 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([N+:21]([O-])=O)=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.CO.[H][H]>[Pd].O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=1

参加物

6

反応物 3

HCID 887MethanolHCID 51346571-(4-Methoxyphenyl)-4-(4-nitrophenyl)piperazineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 154406Benzenamine, 4-(4-(4-methoxyphenyl)-1-piperazinyl)-収率 74%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 12 parts of 1-(4-methoxyphenyl)-4-(4-nitrophenyl)piperazine, 200 parts of methanol and 225 parts of tetrahydrofuran is hydrogenated at normal pressure and at room temperature with 2 parts of palladium-on-charcoal catalyst 10%. After the calculated amount of hydrogen is taken up, the catalyst is filtered off and washed with N,N-dimethylacetamide. The filtrate is poured onto water. The precipitated product is filtered off and crystallized from 1-butanol, yielding 8 parts (74%) of 4-[4-(4-methoxyphenyl)-1-piperazinyl]benzenamine; mp. 191.8° C.

後処理

  1. filtrationthe catalyst is filtered off
  2. washwashed with N,N-dimethylacetamide
  3. additionThe filtrate is poured onto water
  4. filtrationThe precipitated product is filtered off
  5. customcrystallized from 1-butanol

出典と根拠

ORDレコード
ord-a99c23d6cbbe4ed58f1b2c5e700effd9
出典データセット
uspto-grants-1983_01
特許番号
US04368200

関連ノート

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