반응 #1838

ord-a19347c988eb4c1c9861adc66fd17858

반응 방정식

O=[N+]([O-])O
nitric acid
O=S(=O)(O)O
sulfuric acid
O=C(O)c1cccc(OC(F)(F)F)c1
3-trifluoromethoxybenzoic acid
O=C(O)c1cc(OC(F)(F)F)ccc1[N+](=O)[O-]
2-Nitro-5-trifluoromethoxybenzoic acid

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while cooling
  2. 2
    온도The reaction mixture was heated at 50°-55° C. for 1 hour
  3. 3
    온도after cooling
  4. 4
    workup.ADDITIONwas poured onto ice
  5. 5
    여과the residue was filtered off with suction
  6. 6
    기타to give
  7. 7
    기타after drying
  8. 8
    기타8.8 g of product, melting point 90°-93° C. (sintering at 85° C.)

실험 절차

29.7 ml of nitric acid were added dropwise to 76.5 ml of concentrated sulfuric acid, while cooling and stirring, and 9.0 g (43.7 mmol) of 3-trifluoromethoxybenzoic acid were then added. The reaction mixture was heated at 50°-55° C. for 1 hour and, after cooling, was poured onto ice, and the residue was filtered off with suction to give, after drying, 8.8 g of product, melting point 90°-93° C. (sintering at 85° C.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726305uspto-grants-1998_03