HRID2410117

反应详情

EQUATION

反应方程式

HRID 2410117 的结构方程式

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

The stirred mixture of (Z)-3-dimethylamino-2-isocyano-acrylic acid ethyl ester (17.0 g, 100 mmol) and cyclopropylamine (17.21 g, 300 mmol) was heated for 5 h at 75° C. The reaction mixture was cooled to rt and concentrated. Purification of the residue by flash chromatography (EtOAc/hexane, 5:1) gave the title compound as an orange oil. tR: 0.61 min (LC-MS 2); ESI-MS: 181.2 [M+H]+ (LC-MS 2); 1H-NMR (DMSO-d6, 400 MHz) δ ppm 7.85 (s, 1H), 7.79 (s, 1H), 4.18 (q, 2H), 3.55 (m, 1H), 1.23 (t, 3H), 0.91-1.02 (m, 4H).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to rt
  2. concentrationconcentrated
  3. customPurification of the residue by flash chromatography (EtOAc/hexane, 5:1)