Tetrahydrofuran 2-propanol → (3-amino-1-trityl-1H-indazol-5-yl)(3,5-difluorophenyl)methanone

HRID 571892노트

반응식

HRID 571892 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:42]=[C:43]([F:45])[CH:44]=1)[C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[N:12]([C:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[N:11]=[C:10]2[NH:35]C(=O)C(F)(F)F)=[O:6].C(O)(C)C.O1CCCC1>C(N(CC)CC)C>[NH2:35][C:10]1[C:9]2[C:13](=[CH:14][CH:15]=[C:7]([C:5]([C:4]3[CH:42]=[C:43]([F:45])[CH:44]=[C:2]([F:1])[CH:3]=3)=[O:6])[CH:8]=2)[N:12]([C:16]([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)([C:29]2[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:11]=1

참가 물질

4

반응물 2

HCID 22597222Tetrahydrofuran 2-propanolHCID 86647614N-(5-(3,5-Difluorobenzoyl)-1-trityl-1H-indazol-3-yl)-2,2,2-trifluoroacetamide

생성물 1

HCID 68670918(3-amino-1-trityl-1H-indazol-5-yl)(3,5-difluorophenyl)methanone수율 99%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

N-[5-(3,5-Difluoro-benzoyl)-1-trityl-1H-indazol-3-yl]-2,2,2-trifluoro-acetamide (6.12 g, 10 mmol) was heated at 100° C. in a mixture isopropanol/tetrahydrofuran 8:2 (100 mL) and triethylamine (12.2 mL) for 48 hours. The volatiles were partially evaporated and the resulting mixture cooled and filtered. The solid was washed with diethyl ether. After drying under vacum at 70° C. the title compound was obtained as a white solid (5.1 g, 99% yield).

후처리

  1. customThe volatiles were partially evaporated
  2. temperaturethe resulting mixture cooled
  3. filtrationfiltered
  4. washThe solid was washed with diethyl ether
  5. dry with materialAfter drying under vacum at 70° C. the title compound

출처 및 근거

ORD 기록
ord-0a66d1b9007945dc8a86aedc6014fea3
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029356B2

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