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Iodine chloride → 4-(2-Fluoro-4-iodophenylamino)-indazole-1,5-dicarboxylic acid di-tert-butyl ester

HRID 79023
ノート
印刷プレビュー

反応式

HRID 79023 の反応式
[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[C:12]([NH:24][C:25]3[CH:30]=[CH:29][C:28]([Si](C)(C)C)=[CH:27][C:26]=3[F:35])[C:13]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[CH:14][CH:15]=2)[CH:10]=[N:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[I:36]Cl>C(Cl)Cl.S([O-])([O-])(=O)=S.[Na+].[Na+]>[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[C:12]([NH:24][C:25]3[CH:30]=[CH:29][C:28]([I:36])=[CH:27][C:26]=3[F:35])[C:13]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[CH:14][CH:15]=2)[CH:10]=[N:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24640Iodine chlorideHCID 575231194-(2-Fluoro-4-trimethylsilanylphenylamino)-indazole-1,5-dicarboxylic acid di-tert-butyl ester

生成物 1

HCID 670838794-(2-Fluoro-4-iodophenylamino)-indazole-1,5-dicarboxylic acid di-tert-butyl ester収率 52%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒2 回HCID 24477
Sodium Thiosulfate
溶媒

反応条件

温度
0 °C

実験手順

To a solution of 4-(2-fluoro-4-trimethylsilanylphenylamino)-indazole-1,5-dicarboxylic acid di-tert-butyl ester (1.07 g, 2.14 mmol) in DCM (10 mL) at 0° C. was added iodine monochloride as a solution in DCM (4.2 mL, 1N, 4.2 mmol). The reaction mixture was stirred at 0° C. for 20 minutes then diluted with saturated aqueous sodium thiosulfate solution (10 mL) and extracted with DCM (2×10 mL). The combined organic extracts were washed with brine (20 mL), dried (MgSO4) and concentrated in vacuo. The resultant residue was subjected to flash chromatography (Si—PPC, gradient 0-100% DCM in cyclohexane) to yield the title compound as a pale brown solid (611 mg, 52%). LCMS (Method B): RT=5.48 min, [M+H]+=554.

後処理

  1. extractionextracted with DCM (2×10 mL)
  2. washThe combined organic extracts were washed with brine (20 mL)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-c09f80ba895c4cbaad6e7c071c087e60
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841462B2

反応ノート

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