반응 #526884

ord-4e5f265da3054ef0a48a71dc13ae0239

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The precipitate was removed by s filtration
  2. 2
    세척The filtrate was washed with water (2×150 ml) and brine
  3. 3
    건조dried with magnesium sulfate
  4. 4
    기타Removal of the ethyl acetate in vacuo

실험 절차

To a suspension of 6-octyloxy-2-naphthoic acid (3.15 g, 10.5 mmol) and dicyclohexylcarbodiimide in ethyl acetate (25 ml) at 0° C. was added pentafluorophenol (2.12 g, 11.5 mmol). The mixture was stirred at 25° C. for a period of 18 h. The precipitate was removed by s filtration. The filtrate was washed with water (2×150 ml) and brine and dried with magnesium sulfate. Removal of the ethyl acetate in vacuo gave 5.4 g of pentafluorphenyl 6-octyloxy-2-naphthoate as a solid: 1H NMR (400 MHz, CH3OD) δ 0.88 (t, 3, J=6.9 Hz), 4.10 (t, 2, J=6.6 Hz), 7.16 (d, 1), 7.21 (d, 1), 7.80 (d, 1), 7.87 (d,1), 8.08 (dd, 1), 8.69 (d, 1).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05516756uspto-grants-1996_05