HRID339794

反应详情

EQUATION

反应方程式

HRID 339794 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A 200 mL stainless steel Parr vessel was loaded with 5-amino-4,6-dichloro-2-methylpyrimidine (7.2 g, 40 mmol) and 2 M ammonia in isopropanol (100 mL), and then was sealed and heated at 150° C. for 16 h. HPLC analysis indicated complete conversion. The mixture was concentrated in vacuo, and the residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL). This was stirred at 50° C. for 1 h and then was cooled to room temperature. The precipitate was collected by suction filtration, washed sparingly with isopropanol, then air dried on the filter to afford 6-chloro-4,5-diamino-2-methylpyrimidine (5.8 g, 91%) as a brown powder, which was used without further purification in the next step.

WORKUP

后处理

  1. customwas sealed
  2. concentrationThe mixture was concentrated in vacuo
  3. additionthe residue was suspended in a mixture of H2O (10 mL) and isopropanol (35 mL)
  4. temperaturewas cooled to room temperature
  5. filtrationThe precipitate was collected by suction filtration
  6. washwashed sparingly with isopropanol
  7. customair dried on the
  8. filtrationfilter