반응 #1095856

ord-b934f1c3a0624412af5bbd8ceb26b77c

반응 방정식

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
수율 95.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture was extracted with tert-butyl methyl ether three times
  2. 2
    세척The organic layers were washed with a saturated sodium chloride aqueous solution
  3. 3
    건조dried over anhydrous magnesium sulfate
  4. 4
    농축concentrated

실험 절차

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)).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07973028B2uspto-grants-2011_07