반응 #94997

ord-61635044421b488eb86f93ade7559371

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
CCN(CC)CC
triethylamine
CN(C)C(=S)Cl
dimethylthiocarbamoyl chloride
Cc1cc(OC(=S)N(C)C)nc(C(Cl)(Cl)Cl)n1
product
수율 55.0%
Cc1cc(OC(=S)N(C)C)nc(C(Cl)(Cl)Cl)n1
6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Dimethylthiocarbamate
수율 55.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed 16 hours
  2. 2
    여과A trace of dark solid was filtered out
  3. 3
    기타the solution was evaporated on a steam bath
  4. 4
    기타to give a solid residue
  5. 5
    추출This residue was extracted with hot ligroin

실험 절차

A mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.6 g (0.025 mole) triethylamine, 3.2 g (0.025 mole) dimethylthiocarbamoyl chloride, and 100 ml ether was refluxed 16 hours. A trace of dark solid was filtered out and the solution was evaporated on a steam bath to give a solid residue. This residue was extracted with hot ligroin to yield 4.3 g (55% yield) of product (mp 81°-83° C.) on cooling. The structure was confirmed via infrared and elemental analysis.

출처

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