Methyl iodide → N-(2-Bromo-pyridin-3-yl)-4-fluoro-N-methyl-benzenesulfonamide

HRID 1716282ノート

反応式

HRID 1716282 の反応式
[Br:1][C:2]1[C:7]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:19]([O-])([O-])=O.[Cs+].[Cs+].IC>CN(C=O)C.CCOC(C)=O>[Br:1][C:2]1[C:7]([N:8]([CH3:19])[S:9]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:6][CH:5]=[CH:4][N:3]=1

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 86619934N-(2-Bromo-pyridin-3-yl)-4-fluoro-benzenesulfonamide

生成物 1

HCID 86619935N-(2-Bromo-pyridin-3-yl)-4-fluoro-N-methyl-benzenesulfonamide

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of N-(2-bromo-pyridin-3-yl)-4-fluoro-benzenesulfonamide (0.3 g, 0.9 mmol) from Step A in DMF (4 ml) was added Cs2CO3 (0.4 g, 1.3 mmol). To the mixture iodomethane (0.128 ml, 2 mmol) was added at room temperature. The mixture was stirred for 5 hours and then was diluted with EtOAc and washed with saturated NaCl solution. The organic phase was dried over sodium sulfate and concentrated. The crude was purified through Chromatography. (3-4% EtOAc in dichloromethane). MS 344.9 (M+H)+

後処理

  1. washwashed with saturated NaCl solution
  2. dry with materialThe organic phase was dried over sodium sulfate
  3. concentrationconcentrated
  4. customThe crude was purified through Chromatography

出典と根拠

ORDレコード
ord-b0fcd8dbdc56448a835c3b1e8816b0e2
出典データセット
uspto-grants-2010_09
特許番号
US07803793B2

反応ノート

読み込み中…