HRID573548

反应详情

EQUATION

反应方程式

HRID 573548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of ethyl 4-amino-2-bromo-6-methyl-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridine-5-carboxylate (700 mg, 1.661 mmol) (Description 15) in DMSO (7 mL) and aqueous NaOH (2M) (4.15 mL, 8.31 mmol) was heated at 150° C. for 1 h. The mixture was cooled to RT, diluted with water (20 mL) and acidified with formic acid to pH 6. The mixture was then extracted with ethyl acetate (5×30 mL) and the combined organics washed with brine (2×30 mL), dried and concentrated, to give the title compound (513 mg). LCMS (A) m/z: 393/395 [M+1]+, Rt 1.04 min (acidic).

WORKUP

后处理

  1. temperatureThe mixture was cooled to RT
  2. extractionThe mixture was then extracted with ethyl acetate (5×30 mL)
  3. washthe combined organics washed with brine (2×30 mL)
  4. customdried
  5. concentrationconcentrated