반응 #1884950

ord-b722c55349404530850dc330961f8ec3

반응 방정식

COc1ccc(N)cc1
p-Anisidine
c1ccncc1
pyridine
O=C(Cl)c1ccc([N+](=O)[O-])cc1
4-nitrobenzoyl chloride
O
water
COc1ccc(C(=O)Nc2ccc([N+](=O)[O-])cc2)cc1
4-Methoxy-4′-nitrobenzanilide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the precipitate was collected with filtrate under vacuum pressure
  2. 2
    세척washed with 5% sodium bicarbonate (2×10 ml)
  3. 3
    기타The product was used in the next step without further purification

실험 절차

p-Anisidine (1.0 g, 8.1 mmol) was dissolved in anhydrous pyridine (15 ml), 4-nitrobenzoyl chloride (1.5 g, 8.1 mmol) was added. The reaction mixture was allowed to stand at room temperature for 16 hrs. The reaction mixture was poured into water and the precipitate was collected with filtrate under vacuum pressure and washed with 5% sodium bicarbonate (2×10 ml). The product was used in the next step without further purification. 1HNMR (300 MHz, DMSO-d6) δ: 10.46(s, 1H, NH), 8.37(d, J=5.5 Hz, 2H, H-3′,5′), 8.17(d, J=6.3 Hz, 2H, H-2′,6′), 7.48(d, J=6.6 Hz, 2H), 6.97(d, J=6.5 Hz, 2H), 3.75(s, 3H, MeO).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08343457B2uspto-grants-2013_01