HRID450122

反应详情

EQUATION

反应方程式

HRID 450122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 1 hour
  3. customcarefully quenched by the addition of water (5 mL)
  4. additionThe reaction mixture was diluted with aqueous hydrochloric acid (2 mL, 1M)
  5. extractionextracted with ethyl acetate (3×10 mL)
  6. washThe combined organic fractions were washed with brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo