HRID845585

反应详情

EQUATION

反应方程式

HRID 845585 的结构方程式

PROCEDURE

实验过程

The reaction of hydroxylamine 82 (0.71 g, 2 mmol) with 2-nitrobenzaldehyde (59) (0.302 g, 2 mmol) afforded, after workup, a yellow oil. The crude product was purified by flash chromatography with 3:4 ethyl acetate/petroleum ether as the eluant to obtain 0.71 g (1.44 mmol. 72%) of 84 as a yellow oil. The oil crystallized from ether/petroleum ether to yield yellow crystalline solid: mp 130°-132° C.; IR (CH2Cl2) 3440, 2980, 1700, 1625, 1575, 1528, 1470, 1345, 1300, 1215, 1105, 905, 852, 775 cm-1 ; 1H NMR (CDCl3) δ 1.13 (d, J=6.2 Hz, 3H), 1.25 (d, J=6.2 Hz, 3H), 2.31 (s, 6H), 3.66 (s, 3H), 4.97 (septet, J=6.2 Hz, 1H), 5.06 (s, 1H), 6.23 (s, 1H), 7.30-9.31 (m, 9H); 13C NMR (CDCl3) δ 19.98, 20.02, 22.47, 22.72, 40.34, 51.67, 67.85, 103.69, 104.37, 120.22, 121.84, 125.25, 125.61, 128.97, 129.17, 130.11, 131.01, 131.08, 134.11, 145.29, 145.82, 148.17, 149.75, 150.35, 167.43, 168.46. Anal. Calcd for C26H27N3O7 : C, 63.28; H, 5.47. Found: C, 63.18; H, 5.26.

WORKUP

后处理

  1. customafforded
  2. customThe crude product was purified by flash chromatography with 3:4 ethyl acetate/petroleum ether as the eluant