HRID573547

反应详情

EQUATION

反应方程式

HRID 573547 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of ethyl 4-amino-6-methyl-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridine-5-carboxylate (865 mg, 2.53 mmol) (Description 14) in DCM (18 mL), was added N-bromosuccinimide (540 mg, 3.03 mmol) and the resulting mixture stirred for 45 min at RT. The mixture was concentrated and purified by chromatography on silica gel, eluting with a gradient of 0-20% ethyl acetate in cyclohexane, to give the title compound (1.02 g). LCMS (A) m/z: 421/423 [M+1]+, Rt 1.57 min (acidic).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. custompurified by chromatography on silica gel
  3. washeluting with a gradient of 0-20% ethyl acetate in cyclohexane