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

HRID 1186574ノート

反応式

HRID 1186574 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-19fa42c8fd894f068b44498e1e19a950
出典データセット
uspto-grants-2014_03
特許番号
US08673893B2

反応ノート

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