HRID2076127
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
A suspension of 5-(2-methoxy-4-nitro-phenyl)-2-methyl-thiazole (330 mg, 1.32 mmol) and anhydrous stannous chloride (1.28 g, 6.59 mmol) in ethanol (21 mL) was stirred at reflux for 1 hour. The yellow solution is evaporated and the residue dissolved in ethyl acetate. This solution is washed twice with 2N aqueous sodium hydroxide solution, with brine, dried with magnesium sulfate and evaporated to dryness to afford the title compound (266 mg, 91%) as an orange solid. MS ISP (m/e): 221.2 (100) [(M+H)]. 1H NMR (CDCl3, 300 MHz): δ(ppm)=7.81 (s, 1H), 7.33 (d, 1H), 6.31 (m, 2H), 3.87 (s, 3H), 3.83 (m, 2H), 2.69 (s, 3H). mp 125-129° C.
WORKUP
后处理
- temperatureat reflux for 1 hour
- customThe yellow solution is evaporated
- dissolutionthe residue dissolved in ethyl acetate
- washThis solution is washed twice with 2N aqueous sodium hydroxide solution, with brine
- dry with materialdried with magnesium sulfate
- customevaporated to dryness