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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of 7-Chloro-thieno[3,2-b]pyridine-2-carbothioic acid methoxymethyl-amide (93.9 g, 344 mmol) and 900 mL THF was added 1 N HCl (344 mL, 344 mmol). The reaction mixture was heated to reflux for seventy-two hours. The reaction mixture was cooled to 0° C., and 300 mL of concentrated NH4OH was added and stirred. The THF was removed under reduced pressure and the residue was suspended in ethyl acetate and stirred. The precipitate was filtered, washed with ethyl acetate and dried to give 7-chloro-thieno[3,2-b]pyridine-2-carbothioic acid amide (66.7 g) in 85% yield. C8H5ClN2S2: APCI m/z: 228.9/230.9 (MH+); 1H NMR (d6-DMSO): δ 10.24 (s, 1H), 9.94 (s, 1H), 8.65 (d, 1H, J=5.0 Hz), 8.19 (s, 1H), 7.62 (d, 1H, J=5.0 Hz) ppm.
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux for seventy-two hours
- customThe THF was removed under reduced pressure
- stirringstirred
- filtrationThe precipitate was filtered
- washwashed with ethyl acetate
- customdried