HRID1285082

反应详情

EQUATION

反应方程式

HRID 1285082 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6.4 g of the product from Example 3, 0.69 g, 10% palladium-on-carbon catalyst, and 3 ml of concentrated hydrochloric acid in 140 ml methanol was shaken under an atmosphere of hydrogen at 50 p.s.i. on a Parr Hydrogenation Apparatus. After approximately 4 hours, the solution was filtered through a pad of Celite and the filtrate was concentrated in vacuo. The residue was diluted with water and, after being washed with several small portions of ether, the aqueous layer was made strongly basic to pH paper by the addition of 50% sodium hydroxide solution with ice-water cooling. A yellow solid precipitated from the basic solution and was isolated by filtration. Drying in vacuo for 24 hours gave 2.4 g of 2-aminomethyl-4,6-dimethoxy-1,3,5-triazine as a light yellow solid.

WORKUP

后处理

  1. filtrationthe solution was filtered through a pad of Celite
  2. concentrationthe filtrate was concentrated in vacuo
  3. additionThe residue was diluted with water
  4. washafter being washed with several small portions of ether
  5. additionby the addition of 50% sodium hydroxide solution with ice-water cooling
  6. customA yellow solid precipitated from the basic solution
  7. customwas isolated by filtration
  8. customDrying in vacuo for 24 hours