반응 #336595

ord-2f9d5849b1294e929f2a8d44a99c9403

반응 조건

온도
22°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축It was then concentrated under reduced pressure
  2. 2
    기타crystallized
  3. 3
    여과the product was filtered off with suction
  4. 4
    세척washed with petroleum ether

실험 절차

3.6 g (0.015 mol) of 2-carbomethoxybenzenesulfonyl isocyanate in 4 ml of 1,2-dichloroethane were added over the course of 5 minutes to a stirred mixture of 3.15 g (0.015 mol) of 2-amino-4-methoxy-6-trifluoromethoxy-1,3,5-triazine and 150 ml of 1,2-dichloroethane at 22° C., and the mixture was stirred at 22° C. for 12 hours. It was then concentrated under reduced pressure and crystallized using 1:1 methyl tert-butyl ether/petroleum ether, and the product was filtered off with suction and washed with petroleum ether to yield 5.1 g (75.4% of theory) of the title compound of melting point 149° C. (decomposition).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05214143uspto-grants-1993_05