반응 #3197

ord-11cb73d43db14970822d1f7987ae94cd

반응 방정식

Nc1cccc(Cl)c1C(=O)O
2-amino-6-chlorobenzoic acid
O=C(OC(Cl)(Cl)Cl)OC(Cl)(Cl)Cl
bis(trichloromethyl)carbonate
O=c1[nH]c2cccc(Cl)c2c(=O)o1
title compound
O=c1[nH]c2cccc(Cl)c2c(=O)o1
5-Chloro-2H-3,1-benzoxazine-2,4(1H)-dione

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the precipitate was collected by filtration
  2. 2
    세척washed with ether
  3. 3
    기타Air drying

실험 절차

To a stirred warm (50° C.) solution of 2-amino-6-chlorobenzoic acid (2.00 g, 11.7 mM) in tetrahydrofuran (20 mL) was added bis(trichloromethyl)carbonate (1.20 g, 4.10 mM). A vigorous gas evolution ensued along with the formation of a precipitate. The reaction mixture was allowed to cool to room temperature and the precipitate was collected by filtration and washed with ether. Air drying gave the title compound as a tan solid (2.0 g, 87%); MS(CI): 198 (M+H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733910uspto-grants-1998_03