反应 #42795

ord-c0794d0d8fe54a99b7d331cf51b7d0e9

反应方程式

CC#CCOc1ncnc(Cl)c1F
4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine
CC1CCC(C)N1
2,5-dimethylpyrrolidine
[Cl-].[NH4+]
ammonium chloride
CC#CCOc1ncnc(N2C(C)CCC2C)c1F
4-(2-butynyloxy)-5-fluoro-6-(2,5-dimethyl-1-pyrrolidinyl)pyrimidine
收率 95.2%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    萃取the mixture was extracted with tert-butyl methyl ether three times
  2. 2
    洗涤The organic layers were washed with a saturated sodium chloride aqueous solution
  3. 3
    干燥dried over anhydrous magnesium sulfate
  4. 4
    浓缩concentrated

实验过程

0.2 g of 4-(2-butynyloxy)-6-chloro-5-fluoropyrimidine and 0.30 g of 2,5-dimethylpyrrolidine were mixed and left for 18 hours at room temperature. Into the reaction mixture was added a saturated ammonium chloride aqueous solution, and the mixture was extracted with tert-butyl methyl ether three times. The organic layers were washed with a saturated sodium chloride aqueous solution, dried over anhydrous magnesium sulfate and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.25 g of 4-(2-butynyloxy)-5-fluoro-6-(2,5-dimethyl-1-pyrrolidinyl)pyrimidine (hereinafter, referred to as Compound (6)).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07732448B2uspto-grants-2010_06