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1,4-Butanediol → 5-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide

HRID 2382713
ノート
印刷プレビュー

反応式

HRID 2382713 の反応式
[CH2:1]([OH:6])[CH2:2][CH2:3][CH2:4][OH:5].[H-].[Na+].[Br:9][C:10]1[C:11]([Cl:28])=[CH:12][C:13](F)=[C:14]([S:16]([N:19]([CH3:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)(=[O:18])=[O:17])[CH:15]=1>CN(C=O)C>[Br:9][C:10]1[C:11]([Cl:28])=[CH:12][C:13]([O:5][CH2:4][CH2:3][CH2:2][CH2:1][OH:6])=[C:14]([S:16]([N:19]([CH3:26])[C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)(=[O:17])=[O:18])[CH:15]=1
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 3

HCID 80641,4-ButanediolHCID 24758Sodium hydrideHCID 684721885-bromo-4-chloro-2-fluoro-N-methyl-N-pyridin-2-yl-benzenesulfonamide

生成物 1

HCID 684685195-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide収率 96.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
50 °C

実験手順

To a solution of 1,4-butanediol (0.315 mL, 3.6 mmol) in DMF (2.5 mL) at ambient temperature was added sodium hydride (60%, 34 mg, 0.85 mmol) and the mixture was stirred for 15 minutes. A solution of 5-bromo-4-chloro-2-fluoro-N-methyl-N-pyridin-2-yl-benzenesulfonamide (0.268 g, 0.71 mmol) in DMF (2.5 mL) was added and the mixture heated at 50° C. for 2 h. The solvent was removed in vacuo and water and DCM were added. The mixture was extracted with DCM. The organic layer was washed with brine and was dried over anhydrous MgSO4. Concentration of the filtrate provided a residue that was purified by silica gel chromatography [eluent: 50% ethyl acetate in hexane] to afford 5-bromo-4-chloro-2-(4-hydroxy-butoxy)-N-methyl-N-pyridin-2-yl-benzenesulfonamide as a solid (0.309 g). MS: 451.0 (M+H)+; tR=2.59 min (method 1).

後処理

  1. customThe solvent was removed in vacuo and water and DCM
  2. additionwere added
  3. extractionThe mixture was extracted with DCM
  4. washThe organic layer was washed with brine
  5. dry with materialwas dried over anhydrous MgSO4
  6. customConcentration of the filtrate provided a residue that
  7. customwas purified by silica gel chromatography [eluent: 50% ethyl acetate in hexane]

出典と根拠

ORDレコード
ord-663c6000ddc741a292521aeb4fe61ebc
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263588B2

反応ノート

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