HRID4752

反应详情

EQUATION

反应方程式

HRID 4752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 100 ml of ethanol are added 8.8 g (0.025 mole) of 3-{2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]phenyl}-2-propenoic acid to produce a solution which is added to a pressure bottle and flushed with nitrogen. To the solution is added 1 g of 10% palladium on carbon. The pressure bottle is placed in a hydrogenation apparatus and pressurized to 1384 g/cm2 (50 lbs/in.2) with hydrogen. The pressure bottle is shaken until the pressure ceases dropping. The resulting solution is vented, filtered and evaporated at reduced pressure to obtain a residual solid which is recrystallized from chlorobutane o give 7.0 gm of 2-methoxy-4-[2,2,2-trifluoro-1-hydroxy-1-(trifluoromethyl)ethyl]benzenepropanoic acid having a melting point of 116°-117°.

WORKUP

后处理

  1. customto produce a solution which
  2. additionis added to a pressure bottle
  3. customflushed with nitrogen
  4. additionTo the solution is added 1 g of 10% palladium on carbon
  5. filtrationfiltered
  6. customevaporated at reduced pressure
  7. customto obtain a residual solid which
  8. customis recrystallized from chlorobutane