Pyridine → Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate

HRID 1164235

反応式

HRID 1164235 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]([NH2:21])=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[C:22](Cl)(=[O:30])[O:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.N1C=CC=CC=1.O(C(C)C)C(C)C>O.ClCCl>[C:24]1([O:23][C:22](=[O:30])[NH:21][C:18]2[CH:19]=[CH:20][C:15]([N:12]3[CH2:13][CH2:14][N:9]([C:6]4[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=4)[CH2:10][CH2:11]3)=[CH:16][CH:17]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

7

反応物 4

HCID 1049PyridineHCID 7914Diisopropyl EtherHCID 15891Phenyl chloroformateHCID 154406Benzenamine, 4-(4-(4-methoxyphenyl)-1-piperazinyl)-

生成物 1

HCID 981607Phenyl N-(4-(4-(4-methoxyphenyl)piperazin-1-yl)phenyl)carbamate収率 61%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 6 parts of 4-[4-(4-methoxyphenyl)-1-piperazinyl]benzenamine, 3.6 parts of phenyl carbonochloridate, 75 parts of pyridine and 98 parts of dichloromethane is stirred and warmed till all solid enters solution. Stirring is continued for 30 minutes at room temperature. The reaction mixture is poured onto 500 parts of water and 210 parts of 2,2'-oxybispropane are added. The whole is stirred for a while. The precipitated product is filtered off and crystallized from 1-butanol, yielding 5.2 parts (61%) of phenyl{4-[4-(4-methoxyphenyl)-1-piperazinyl]phenyl}carbamate; mp. 204.5° C.

後処理

  1. temperaturewarmed till all solid
  2. stirringStirring
  3. additionare added
  4. stirringThe whole is stirred for a while
  5. filtrationThe precipitated product is filtered off
  6. customcrystallized from 1-butanol

出典と根拠

ORDレコード
ord-c728eed3e3784f39854ff3fd7bdb9062
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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