18-Crown-6 → 3-Chloro-4-fluorobenzenesulfonyl fluoride
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([S:9](Cl)(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8].[F-:13].[K+].C1OCCOCCOCCOCCOCCOC1>CC#N>[Cl:1][C:2]1[CH:3]=[C:4]([S:9]([F:13])(=[O:11])=[O:10])[CH:5]=[CH:6][C:7]=1[F:8]参加物
5
実験手順
To a solution of the commercially available 3-chloro-4-fluorobenzenesulfonyl chloride (7 g, 30 mmol) in CH3CN (40 mL) was added KF (7 g, 120 mmol) and 18-crown-6 (0.5 g), then the mixture was stirred at room temperature overnight. The mixture was quenched with aqueous water and extracted with EtOAc, the organic layer was washed with brine, dried over anhydrous Na2SO4, concentrated to give the crude product which was purified by column to give the reagent R-12a (4.2 g, 95.5%) as a pale yellow solid. ESI-MS (M+1): 213.2 calc. for C6H3CIF2O2S
後処理
- customThe mixture was quenched with aqueous water
- extractionextracted with EtOAc
- washthe organic layer was washed with brine
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-4d2f9af19e2e475e8307933b0643585b
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440989B2
反応ノート
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