Diethyl Ether → 1h-Indazole-1-carboxylic acid,5-(azidomethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester

HRID 503132

反応式

HRID 503132 の反応式
Cl[CH2:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[N:7]=[C:6]2[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=1.[N-:26]=[N+:27]=[N-:28].[Na+].C(OCC)C>CS(C)=O>[N:26]([CH2:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[N:7]=[C:6]2[C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([F:25])[CH:20]=1)=[N+:27]=[N-:28]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 33557Sodium AzideHCID 222606161h-Indazole-1-carboxylic acid,5-(chloromethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester

生成物 1

HCID 222608731h-Indazole-1-carboxylic acid,5-(azidomethyl)-3-(3-fluorophenyl)-,1,1-dimethylethyl ester収率 93.5%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

To a solution of 600 mg of tert-butyl 5-(chloromethyl)-3-(3-fluorophenyl)-1H-1-indazolecarboxylate produced in Production Example I-24-b in 4 ml dimethyl sulfoxide was added 162 mg of sodium azide, and the mixture was stirred at room temperature for 50 minutes. To the reaction mixture was added 25 ml of diethyl ether. The mixture was sequentially washed with water (×3) and brine, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 571 mg of the title compound as pale yellow crystals.

後処理

  1. washThe mixture was sequentially washed with water (×3) and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-094a3b4006c0461ba536ac5abb32374a
出典データセット
uspto-grants-2010_08
特許番号
US07776890B2

関連ノート

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