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

HRID 414242

反応式

HRID 414242 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>[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]([NH:21][C:22](=[O:30])[O:23][C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:7][CH:8]=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 was stirred and warmed till all solid entered solution. Stirring was continued for 30 minutes at room temperature. The reaction mixture was poured into 500 parts of water and 210 parts of 2,2'-oxybispropane were added. The whole was stirred for a while. The precipitated product was 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 (intermediate 18).

後処理

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

出典と根拠

ORDレコード
ord-7e34742856264106811cee026c524991
出典データセット
uspto-grants-1988_12
特許番号
US04791111

関連ノート

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