Sodium Carbonate → N-(3-Chloro-6-trifluoromethylimidazo[1,2-a]pyridin-2-yl)-N-(3-fluoro-4-trifluoromethylbenzyl)benzenesulfonamide

HRID 1916858ノート

反応式

HRID 1916858 の反応式
[Cl:1][C:2]1[N:6]2[CH:7]=[C:8]([C:11]([F:14])([F:13])[F:12])[CH:9]=[CH:10][C:5]2=[N:4][C:3]=1[NH:15][S:16]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)(=[O:18])=[O:17].C([O-])([O-])=O.[Na+].[Na+].[F:31][C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][C:39]=1[C:40]([F:43])([F:42])[F:41])[CH2:35]Br>CN(C=O)C>[Cl:1][C:2]1[N:6]2[CH:7]=[C:8]([C:11]([F:12])([F:14])[F:13])[CH:9]=[CH:10][C:5]2=[N:4][C:3]=1[N:15]([CH2:35][C:34]1[CH:37]=[CH:38][C:39]([C:40]([F:41])([F:42])[F:43])=[C:32]([F:31])[CH:33]=1)[S:16]([C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)(=[O:18])=[O:17]

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 27375744-(Bromomethyl)-2-fluoro-1-(trifluoromethyl)benzeneHCID 67953932N-(3-chloro-6-trifluoromethylimidazo[1,2-a]pyridin-2-yl)benzenesulfonamide

生成物 1

HCID 88531008N-(3-Chloro-6-trifluoromethylimidazo[1,2-a]pyridin-2-yl)-N-(3-fluoro-4-trifluoromethylbenzyl)benzenesulfonamide収率 58%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of compound 9-E (0.015 g, 0.025 mmol) in DMF (2.0 mL) was added Na2CO3 (0.011 g, 0.099 mmol) and 3-fluoro-4-trifluoromethylbenzyl bromide (0.006 g, 0.025 mmol). The reaction mixture was stirred at room temperature overnight. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography (SiO2) eluting with a gradient of 0-100% ethyl acetate in hexane to afford Compound 60 (0.008 g, 58%); MS m/z (M+H+) 552.

後処理

  1. customThe solvent was evaporated in vacuo
  2. customthe residue was purified by flash column chromatography (SiO2)
  3. washeluting with a gradient of 0-100% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ec5564d457b9429794b3381fe1bcdc23
出典データセット
uspto-grants-2013_12
特許番号
US08618150B2

反応ノート

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