反应 #44525

ord-ee4c67b25ee64efdb3c0893c80b0defa

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled
  2. 2
    浓缩concentrated
  3. 3
    workup.ADDITIONtreated with water
  4. 4
    萃取extracted with ethyl acetate
  5. 5
    洗涤The extract was washed with brine
  6. 6
    干燥dried over anhydrous sodium sulfate
  7. 7
    浓缩concentrated
  8. 8
    其他The concentrate was triturated with ethyl ether
  9. 9
    过滤filtered

实验过程

A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737159B2uspto-grants-2010_06