반응 #467489

ord-79d96937a5a948a282e05d9a4b55435d

반응 방정식

O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=c1cc(C(F)(F)F)[nH]c(=O)n1-c1cc(Oc2ncccc2[N+](=O)[O-])c(Cl)cc1F
3-[4-chloro-2-fluoro-5-(3-nitro-2-pyridyloxy)phenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione
NOc1ccc([N+](=O)[O-])cc1[N+](=O)[O-]
2,4-dinitrophenoxyamine
Nn1c(C(F)(F)F)cc(=O)n(-c2cc(Oc3ncccc3[N+](=O)[O-])c(Cl)cc2F)c1=O
semi-solid
수율 58.0%
Nn1c(C(F)(F)F)cc(=O)n(-c2cc(Oc3ncccc3[N+](=O)[O-])c(Cl)cc2F)c1=O
1-amino-3-[4-chloro-2-fluoro-5-(3-nitro-2-pyridyloxy)phenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione
수율 58.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the resulting oil chromatographed on silica gel eluting with methanol

실험 절차

A suspension of potassium carbonate (0.23 g), 3-[4-chloro-2-fluoro-5-(3-nitro-2-pyridyloxy)phenyl]-6-trifluoromethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione (0.5 g) and 2,4-dinitrophenoxyamine (0.32 g) in N,N-dimethylformamide (10 ml) was stirred at room temperature overnight. The solution was processed and the resulting oil chromatographed on silica gel eluting with methanol:methylene chloride, 2:98. The product was isolated as a yellow semi-solid (0.3 g), mp 90-6° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06303543B1uspto-grants-2001_10