Chloroform → 5-(3-Benzoylthioureidomethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

HRID 4685

반응식

HRID 4685 반응식
[S-:1][C:2]#[N:3].[NH4+].[C:5](Cl)(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[NH2:14][CH2:15][C:16]1[C:17]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([N+:35]([O-:37])=[O:36])[CH:30]=2)=[N:18][C:19]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:20][C:21]=1[CH3:22].C(Cl)(Cl)Cl>CC(C)=O.O>[C:5]([NH:3][C:2](=[S:1])[NH:14][CH2:15][C:16]1[C:17]([C:29]2[CH:34]=[CH:33][CH:32]=[C:31]([N+:35]([O-:37])=[O:36])[CH:30]=2)=[N:18][C:19]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)=[N:20][C:21]=1[CH3:22])(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

참가 물질

7

반응물 4

HCID 6212ChloroformHCID 7412Benzoyl chlorideHCID 15666Ammonium thiocyanateHCID 201514135-Aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

생성물 1

HCID 540990445-(3-Benzoylthioureidomethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine수율 81%

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 962Water용매

실험 절차

A mixture of ammonium thiocyanate (0.25 g) and benzoyl chloride (0.41 g) in acetone (20 ml) was refluxed for 2 hours, and 5-aminomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (0.9 g) in acetone (5 ml) was added thereto. After refluxing for 2 hours, the reaction mixture was poured into a mixture of chloroform (100 ml) and water (50 ml). The organic layer was separated, washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The solvent was distilled off and the resulting crystal was recrystallized from diisopropyl ether to give 5-(3-benzoylthioureidomethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.1 g).

후처리

  1. temperaturewas refluxed for 2 hours
  2. temperatureAfter refluxing for 2 hours
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was distilled off
  7. customthe resulting crystal was recrystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-bc3a3701e39b42c0a3d5a904d9d85908
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04727073

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