Ammonium Hydroxide → 6-chloropyridine-3-sulfonamide
反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[OH-].[NH4+:13]>CCOC(C)=O>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:13])(=[O:10])=[O:9])=[CH:4][CH:3]=1参加物
4
実験手順
6-chloropyridine-3-sulfonyl chloride (4.1 g, 19.3 mmol) was stirred in ammonium hydroxide (30 mL) at room temperature for 2 hr. The reaction mixture was diluted with EtOAc (150 mL) and any insoluble material filtered. The filtrate was transferred to a separatory funnel and the phases were separated. The aqueous phase was further extracted with EtOAc (1×15 mL). The combined EtOAc extractions were washed with H2O (1×50 mL) and saturated NaCl (1×50 mL), dried over Na2SO4, and concentrated in vacuo to give 6-chloropyridine-3-sulfonamide (2.58 g, 69%). MS (EI) m/z for C5H5Cl2N2O2S: 190.9 (MH+).
後処理
- filtrationany insoluble material filtered
- customThe filtrate was transferred to a separatory funnel
- customthe phases were separated
- extractionThe aqueous phase was further extracted with EtOAc (1×15 mL)
- extractionThe combined EtOAc extractions
- washwere washed with H2O (1×50 mL) and saturated NaCl (1×50 mL)
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-9a6a59e8d2a84947a6d6eac15adc6a6f
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08889664B2
反応ノート
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