Methyl Isocyanate → HCID 21249986, 화합물

HRID 1531654노트

반응식

HRID 1531654 반응식
[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][NH:9][CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1.[CH3:25][N:26]=[C:27]=[O:28]>C(Cl)Cl>[Br:1][C:2]1[C:3]([O:23][CH3:24])=[CH:4][C:5]2[C:11]([C:12]3[CH:17]=[CH:16][C:15]([N+:18]([O-:20])=[O:19])=[CH:14][CH:13]=3)=[N:10][N:9]([C:27](=[O:28])[NH:26][CH3:25])[CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1

참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 21249960HCID 21249960, 화합물

생성물 1

HCID 21249986HCID 21249986, 화합물수율 83.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.60 g (1.5 mmol) of 7-bromo-4-methyl-8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is dissolved in 12 ml of dry methylene chloride and mixed with 0.64 ml (10.5 mmol) of methyl isocyanate. After a reaction period of 9 days at 25° C., the solution is concentrated by evaporation, and the residue is recrystallized from ethanol (10 ml). 0.56 g (83%) of 7-bromo-4-methyl-3-methylcarbamoyl-8-methoxy-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine in the form of yellow crystals with a melting point of 224-226° C. is obtained.

후처리

  1. customAfter a reaction period of 9 days at 25° C.
  2. concentrationthe solution is concentrated by evaporation
  3. customthe residue is recrystallized from ethanol (10 ml)

출처 및 근거

ORD 기록
ord-2a50461554d1498db1a34940bc232bbf
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200970B1

반응 노트

불러오는 중…