Trichloroacetyl chloride → 2,2,2-Trichloro-1-[10-(9H-fluorene-2-carbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-ethanone

HRID 2244298노트

반응식

HRID 2244298 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[C:14]([N:16]1[C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=2[CH2:20][N:19]2[CH:27]=[CH:28][CH:29]=[C:18]2[CH2:17]1)=[O:15].[Cl:30][C:31]([Cl:36])([Cl:35])[C:32](Cl)=[O:33]>O1CCOCC1>[Cl:30][C:31]([Cl:36])([Cl:35])[C:32]([C:27]1[N:19]2[C:18]([CH2:17][N:16]([C:14]([C:2]3[CH:3]=[CH:4][C:5]4[C:6]5[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=5)[CH2:12][C:13]=4[CH:1]=3)=[O:15])[C:22]3[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=3[CH2:20]2)=[CH:29][CH:28]=1)=[O:33]

참가 물질

4

반응물 2

HCID 6420Trichloroacetyl chlorideHCID 6869069310-(9H-Fluoren-2-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine

생성물 1

HCID 686864232,2,2-Trichloro-1-[10-(9H-fluorene-2-carbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl]-ethanone수율 88.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To 25 mL of 1,4-dioxane was added 0.59 g (0.0016 mol) of 10-(9H-fluoren-2-ylcarbonyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine opf Step A followed by the addition of 0.31 g (0.0017 mol) of trichloroacetyl chloride. The solution was heated under reflux for 10 minutes, cooled to room temperature and poured into ice water with stirring The precipitate was collected, washed with water and dried yielding 0.74 g of title compound which was used directly in the next step.

후처리

  1. temperatureThe solution was heated
  2. temperatureunder reflux for 10 minutes
  3. customwas collected
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-8a607f0b468f42d086b8e5b8b9bbd66c
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07678787B2

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