HRID490968

反应详情

EQUATION

反应方程式

HRID 490968 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6.0 g of 5-(4-fluorophenyl)pyridine-3-carboxylic acid morpholinamide from Example 1(b) are dissolved in 30 ml of THF, and 57 g of a 13.6% LiAlH—(OEt)3 solution in THF are added over the course of 10 minutes at 30° C. to 35° C. After 1 hour, 30 ml of 12.5% sulfuric acid are added, and the organic phase is separated off. The aqueous phase is adjusted to pH 1 using sulfuric acid and extracted a number of times with methyl tert-butyl ether. The organic phases are then combined, extracted once with water and then evaporated, leaving a residue of 4.3 g having a content of 97% by weight of 5-(4-fluorophenyl)pyridine-3-carbaldehyde (yield=98% of theory).

WORKUP

后处理

  1. customthe organic phase is separated off
  2. extractionextracted a number of times with methyl tert-butyl ether
  3. extractionextracted once with water
  4. customevaporated
  5. customleaving a residue of 4.3 g