HRID639027
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
- -10 °C
PROCEDURE
实验过程
Methyl 7-methyl-3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylate (54 mg, 0.195 mmol) was dissolved in THF (5 mL), cooled to −10° C. and treated with 1.0M LiH3BNMe2 (0.42 mL, 0.42 mmol). The reaction was maintained at −10° C. for 1 h and then quenched with 6N HCl. The reaction solution was diluted with EtOAc and water and the aqueous phase was extracted with EtOAc. The combined organic phases were dried (Na2SO4), filtered and concentrated. The crude product (30.3 mg) was used directly in the next step without further purification.
WORKUP
后处理
- additiontreated with 1.0M LiH3BNMe2 (0.42 mL, 0.42 mmol)
- temperatureThe reaction was maintained at −10° C. for 1 h
- customquenched with 6N HCl
- additionThe reaction solution was diluted with EtOAc and water
- extractionthe aqueous phase was extracted with EtOAc
- dry with materialThe combined organic phases were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude product (30.3 mg) was used directly in the next step without further purification