반응 #93659

ord-8da94d8fab044e368db50f6bb8487cc1

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척the organic phase is washed with water
  2. 2
    건조After drying over sodium sulphate and removal of the solvent in vacuo
  3. 3
    workup.STIRRINGthe resulting residue is stirred with 100 ml of petroleum ether
  4. 4
    여과filtered off with suction
  5. 5
    세척rinsed with petroleum ether
  6. 6
    기타dried

실험 절차

68.5 g (0.3 mole) of 2,4,6-trichloro-5-methylthiopyrimidine are dissolved in 300 ml of toluene. 30.3 g (0.3 mole) of triethylamine and 35.1 g (0.3 mole) of isopropoxypropylamine are added dropwise at 0° C. After the mixture had been subsequently stirred at room temperature for 1 hour, it is diluted with 500 ml of toluene and the organic phase is washed with water. After drying over sodium sulphate and removal of the solvent in vacuo, the resulting residue is stirred with 100 ml of petroleum ether, filtered off with suction, rinsed with petroleum ether and dried. 25.3 g (27.2% of theory) of the above-mentioned pyrimidine, melting point: 88° C., are thus obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04614532uspto-grants-1986_09