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

HRID 979046노트

반응식

HRID 979046 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2fd9087da28744bb97d7896d2407f40e
출처 데이터셋
uspto-grants-1987_05
특허 번호
US04666911

반응 노트

불러오는 중…