HRID1698508
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-(Propylsulphonyl)benzaldehyde (1.81 g, 8.53 mmol, prepared as described in Example 47a, tert-butyl sulphinamide (1.55 g, 12.8 mmol), titanium(V) ethoxide (3.58 mL, 17.1 mmol) and THF (50 mL) were heated at reflux for 3 h then stirred at room temperature overnight. The reaction mixture was quenched with water (200 mL) before addition of ethyl acetate (200 mL). Celite was added and the mixture stirred for 15 min before being filtered. The phases were separated and the organic extract dried (MgSO4) and concentrated. The yield of the title compound was assumed to be quantitative and the material was used without further purification. m/z (ES+) 316 (M+H).
WORKUP
后处理
- temperaturewere heated
- temperatureat reflux for 3 h
- customThe reaction mixture was quenched with water (200 mL) before addition of ethyl acetate (200 mL)
- additionCelite was added
- stirringthe mixture stirred for 15 min
- filtrationbefore being filtered
- customThe phases were separated
- extractionthe organic extract
- dry with materialdried (MgSO4)
- concentrationconcentrated
- customthe material was used without further purification