HRID450122
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 5-chloro-7-(2-fluoro-4-iodo-phenylamino)-pyrrolo[1,2-c]pyrimidine-6-carboxylic acid methyl ester (300 mg, 0.67 mmol) in DCM (6 mL) was added boron tribromide (0.65 mL, 6.7 mmol). The reaction was heated at reflux for 1 hour. The reaction mixture was cooled to 0° C. and carefully quenched by the addition of water (5 mL). The reaction mixture was diluted with aqueous hydrochloric acid (2 mL, 1M) and extracted with ethyl acetate (3×10 mL). The combined organic fractions were washed with brine, dried (MgSO4) and concentrated in vacuo to give the product as a dark brown solid (335 mg, 115%). LCMS (Method B): RT=3.58 min, M+H+=432.
WORKUP
后处理
- temperatureThe reaction was heated
- temperatureat reflux for 1 hour
- customcarefully quenched by the addition of water (5 mL)
- additionThe reaction mixture was diluted with aqueous hydrochloric acid (2 mL, 1M)
- extractionextracted with ethyl acetate (3×10 mL)
- washThe combined organic fractions were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo