Trityl chloride → N-(5-(3,5-Difluorobenzoyl)-1-trityl-1H-indazol-3-yl)-2,2,2-trifluoroacetamide

HRID 571891ノート

反応式

HRID 571891 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:23]=[C:24]([F:26])[CH:25]=1)[C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[NH:12][N:11]=[C:10]2[NH:16][C:17](=[O:22])[C:18]([F:21])([F:20])[F:19])=[O:6].Cl[C:28]([C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)([C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C(N(CC)CC)C>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([CH:23]=[C:24]([F:26])[CH:25]=1)[C:5]([C:7]1[CH:8]=[C:9]2[C:13](=[CH:14][CH:15]=1)[N:12]([C:28]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1)[C:35]1[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=1)[N:11]=[C:10]2[NH:16][C:17](=[O:22])[C:18]([F:20])([F:21])[F:19])=[O:6]

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 86647613N-(5-(3,5-Difluorobenzoyl)-1H-indazol-3-yl)-2,2,2-trifluoroacetamide

生成物 1

HCID 86647614N-(5-(3,5-Difluorobenzoyl)-1-trityl-1H-indazol-3-yl)-2,2,2-trifluoroacetamide収率 86.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-[5-(3,5-Difluoro-benzoyl)-1H-indazol-3-yl]-2,2,2-trifluoro-acetamide (19.11 g, 51.76 mmol) in dry dichloromethane (300 mL) was treated with chlorotriphenylmethane (14.72 g, 52.8 mmol) and triethylamine (14.55 mL, 103.5 mmol). After stirring at room temperature for two days, the reaction was washed with a solution of NH4Cl, dried and evaporated. Purification of the crude by chromatography over silica gel (DCM/MeOH) afforded 27.32 g of the title compound (86% yield).

後処理

  1. washthe reaction was washed with a solution of NH4Cl
  2. customdried
  3. customevaporated
  4. customPurification of the crude by chromatography over silica gel (DCM/MeOH)

出典と根拠

ORDレコード
ord-52cca342fa76483eac7b8413572f8d16
出典データセット
uspto-grants-2015_05
特許番号
US09029356B2

反応ノート

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