反应 #1124

ord-5a04f014ea6d40c2b125f6974f5951e3

反应方程式

Cl
hydrochloric acid
Clc1nccc(N[C@H]2CC[C@@H](c3ccccc3)CC2)c1Br
2-chloro-3-bromo-4-(cis-4-phenylcyclohexylamino)pyridine
C[O-].[Na+]
sodium methoxide
O
water
COc1nccc(N[C@H]2CC[C@@H](c3ccccc3)CC2)c1Br
2-Methoxy-3-bromo-4-(cis-4-phenylcyclohexylamino)pyridine

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling
  2. 2
    萃取the reaction product is extracted with ethyl acetate
  3. 3
    其他For purification it
  4. 4
    其他is chromatographed

实验过程

2.21 g (6.04 mmol) of 2-chloro-3-bromo-4-(cis-4-phenylcyclohexylamino)pyridine in 30 ml of dimethylformamide are treated with 4.31 ml of 30% strength solution of sodium methoxide in methanol and the mixture is heated at 80° C. for 1 hour. After cooling, water is added, the mixture is adjusted to pH 8 using 1/2 conc. hydrochloric acid and the reaction product is extracted with ethyl acetate. For purification it is chromatographed. Yield: 1.72 g (79%); Rf =0.4 (diisopropyl ether)

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723450uspto-grants-1998_03