HRID2172731

反应详情

EQUATION

反应方程式

HRID 2172731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Methyl 6-(4′-fluoro-[1,1′-biphenyl]-4-yl)-4-vinylpicolinate (600 mg, 1.8 mmol) was dissolved in 10 mL of methanol in a pressure tube. Into the tube was condensed about 10 mL ammonia at −20° C. to −30° C. The pressure tube was tightly closed and the resulting solution was stirred at room temperature for overnight. TLC (silica gel, 10% methanol in chloroform) showed the reaction had gone to completion. The ammonia was removed by nitrogen purge and the methanol was removed under reduced pressure to obtain 300 mg of 6-(4′-fluoro-[1,1′-biphenyl]-4-yl)-4-vinylpicolinamide which was pure enough to take to next step without purification.

WORKUP

后处理

  1. customThe pressure tube was tightly closed
  2. customThe ammonia was removed by nitrogen
  3. custompurge
  4. customthe methanol was removed under reduced pressure