HRID973503
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To tert-butylmercaptan (0.11 ml) in dimethylformamide (5 ml) at 0° C. was added potassium bis(trimethylsilyl)amide in toluene (1.80 ml, 0.90 mmol, 0.5M) followed by the resultant compound from Example 34 (259.6 mg, 0.785 mmol) in dimethylformamide (3 ml). After 16 h at room temperature the mixture was diluted with ethyl acetate, washed with water and brine, then dried over Na2SO4 and evaporated. Chromatography of the residue on silica gel with 10% ethyl acetate in hexane afforded 219.6 mg (73%) of a colorless oil. 1H NMR (CDCl3) δ7.10-7.40 (m,10H), 5.07 (s,2H), 3.25 (s,2H), 3.18-3.29 (m,1H), 2.97-3.07 (m,2H), 2.78 (dd,1H), 2.71 (dd,1H), 1.25 (s,9H).
WORKUP
后处理
- washwashed with water and brine
- dry with materialdried over Na2SO4
- customevaporated