HRID2421841
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
- 70 °C
PROCEDURE
实验过程
To a solution of methyl 3-amino-4-(2-chloroethylthio)benzoate (19.7 mg, 0.080 mmol) in 2-butanone (2 mL) was added sodium iodide (36 mg, 0.240 mmol). The reaction mixture was heated to 70° C. and stirred over night at that temperature. The reaction mixture was cooled to room temperature. TLC and LCMS analysis of the reaction mixture indicated product formation. The product was purified by flash column chromatography [gradient elution with Hexanes and 5-50% EtOAc]. To provide methyl 3,4-dihydro-2H-benzo[b][1,4]thiazine-6-carboxylate (8.6 mg, 0.040 mmol, 49.6% overall 3 steps) as an off-white solid.
WORKUP
后处理
- temperatureThe reaction mixture was cooled to room temperature
- customThe product was purified by flash column chromatography [gradient elution with Hexanes and 5-50% EtOAc]