Water → HCID 68687571, 화합물

HRID 2244216노트

반응식

HRID 2244216 반응식
[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:6]=[CH:5][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[CH:20]=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:3][CH:2]=1.[Cl:29][C:30]([Cl:35])([Cl:34])[C:31](Cl)=[O:32].O>O1CCOCC1>[C:1]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:2]=[CH:3][C:4]([C:7]([N:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH2:13][N:12]3[C:20]([C:31](=[O:32])[C:30]([Cl:35])([Cl:34])[Cl:29])=[CH:21][CH:22]=[C:11]3[CH2:10]2)=[O:8])=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 6420Trichloroacetyl chlorideHCID 9799174HCID 9799174, 화합물

생성물 1

HCID 68687571HCID 68687571, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

10-(1,1′-Biphenyl-4-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine of Step A (1.822 g; 0.005 mol) was dissolved in 50 mL of 1,4-dioxane to which was then added 0.946 g (0.0052 mol) of trichloroacetyl chloride. The reaction solution was heated under reflux with stirring over night, cooled to room temperature and then poured into 250 mL of water. Recrystallization of the crude material from ethanol provided a solid, m.p. 197-198° C.

후처리

  1. temperatureThe reaction solution was heated
  2. temperatureunder reflux
  3. customRecrystallization of the crude material from ethanol
  4. customprovided a solid, m.p. 197-198° C.

출처 및 근거

ORD 기록
ord-e83aa627fea141a297d2ee9749e36791
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678787B2

반응 노트

불러오는 중…