Dichloromethane → 1-Piperazinecarboxamide, N-((methylamino)carbonyl)-4-phenyl-

HRID 979046ノート

反応式

HRID 979046 の反応式
ClCCl.[C:4]1([N:10]2[CH2:15][CH2:14][N:13]([C:16]([NH2:18])=[O:17])[CH2:12][CH2:11]2)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:19][N:20]=[C:21]=[O:22]>O>[CH3:19][NH:20][C:21](=[O:22])[NH:18][C:16]([N:13]1[CH2:12][CH2:11][N:10]([C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH2:15][CH2:14]1)=[O:17]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 12228Methyl IsocyanateHCID 2503654-Phenylpiperazine-1-carboxamide

生成物 1

HCID 30669291-Piperazinecarboxamide, N-((methylamino)carbonyl)-4-phenyl-収率 51.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Into 70 ml of dichloromethane, were dissolved 4.1 g of 4-phenylpiperazine-1-carboxamide and 1.2 g of methyl isocyanate. To the solution, while being stirred and cooled in ice, was added dropwise 5.2 g of stannic chloride. After 15 hours of reaction at room temperature, water was added to separate an organic layer. The organic layer was dried over anhydrous sodium sulfate and freed from the solvent by distillation. The residue was recrystallized from ethanol to obtain 2.7 g (51% yield) of 1-(4-methylallophanoyl)-4-phenylpiperazine having a melting point of 198°-200° C.

後処理

  1. temperaturecooled in ice
  2. customAfter 15 hours of reaction at room temperature
  3. customto separate an organic layer
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. distillationfreed from the solvent by distillation
  6. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-2fd9087da28744bb97d7896d2407f40e
出典データセット
uspto-grants-1987_05
特許番号
US04666911

反応ノート

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