Triethylamine → HCID 21249956, 화합물

HRID 1531658노트

반응식

HRID 1531658 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.C(N(CC)CC)C.[CH:32]1([C:35](Cl)=[O:36])[CH2:34][CH2:33]1>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:35]([CH:32]3[CH2:34][CH2:33]3)=[O:36])[CH:8]([CH3:21])[CH2:7][C:6]=2[CH:22]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 21249960HCID 21249960, 화합물

생성물 1

HCID 21249956HCID 21249956, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

0.69 g (1.77 mmol) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is acylated in methylene chloride (15 ml) in the presence of 0.29 ml (2.1 mmol) of triethylamine with 0.19 ml (2.1 mmol) of cyclopropanoic acid chloride at room temperature for 1.5 hours. After concentration by evaporation and suspension with water, 0.78 g of a crude product, which is purified by suspension in hot ethanol, is obtained. 0.75 g (93%) of 7-bromo-3-cyclopropylcarbonyl-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine with a melting point of 194-196° C. is obtained.

후처리

  1. concentrationAfter concentration
  2. customby evaporation and suspension with water, 0.78 g of a crude product, which
  3. customis purified by suspension in hot ethanol
  4. customis obtained

출처 및 근거

ORD 기록
ord-7c60cf63ded243b0bfd61274c4f0a350
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200970B1

반응 노트

불러오는 중…