반응 #95003

ord-c92a06f657304b658322e781547f7510

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(Cl)N1CCCC1
pyrrolidinecarbonyl chloride
Cc1cc(C(=O)ON2CCCC2)nc(C(Cl)(Cl)Cl)n1
residue
수율 125.8%
Cc1cc(C(=O)ON2CCCC2)nc(C(Cl)(Cl)Cl)n1
6-Methyl-4-(1-Pyrrolidinylcarboxy)-2-Trichloromethylpyrimidine
수율 125.8%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed 5.3 hours
  2. 2
    여과A precipitate was filtered out
  3. 3
    기타the filtrate rotary evaporated

실험 절차

A mixture of 5.8 g (0.027 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 3.3 g (0.024 mole) potassium carbonate, 3.2 g (0.024 mole) pyrrolidinecarbonyl chloride, and 100 ml acetone was refluxed 5.3 hours. A precipitate was filtered out and the filtrate rotary evaporated to give 9.8 g residue. This was taken up in chloroform, the solution washed with 1% sodium hydroxide, water, and dried over anhydrous magnesium sulfate. Rotary evaporation yielded 4.4 g residue which was recrystallized from petroleum ether to give 2.2 g (28% yield; mp 93°-95° C.) of product. The structure was confirmed via infrared and elemental analysis.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04343803uspto-grants-1982_08