HRID356646

反应详情

EQUATION

反应方程式

HRID 356646 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.09 g of 4,6-dichloro-5-(2-methoxy-phenoxy)-2,2'-bipyrimidine (EP-A- 0 526 708) were suspended in 75 ml of methanol and 150 ml of ammonia were condensed at 75° C. using a feedpipe. The reaction mixture was left to come to room temperature overnight, concentrated in a water-jet vacuum and the residue was partitioned between a small amount of water and methylene chloride (500 ml). The organic phase was dried over sodium sulphate and concentrated on a rotary evaporator. The residue was triturated with ether, the resulting solid was separated and dried in a high vacuum. The 4-amino-6-chloro-5-(2-methoxy-phenoxy )-2,2'-bipyrimidine was thus obtained as a fine, almost white powder. MS: 329 (M).

WORKUP

后处理

  1. customcondensed at 75° C.
  2. waitThe reaction mixture was left
  3. concentrationconcentrated in a water-jet vacuum
  4. customthe residue was partitioned between a small amount of water and methylene chloride (500 ml)
  5. dry with materialThe organic phase was dried over sodium sulphate
  6. concentrationconcentrated on a rotary evaporator
  7. customThe residue was triturated with ether
  8. customthe resulting solid was separated
  9. customdried in a high vacuum