HRID1820114

反应详情

EQUATION

反应方程式

HRID 1820114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Bromo-2,6-dichloroaniline (12.1 g) and cyclopentylacetyl chloride (8.1 g) were dissolved in tetrahydrofuran (100 mL) and sodiumcarbonate (6.4 g) is added, followed by heating to reflux for 6 hours. The reaction mixture was cooled to ambient temperature and filtered and diluted with water (250 ml). After extraction, the combined organic phase was concentrated in vacuo to furnish 14.0 g (80% yield) of the title compound as a white solid. LC-MS (m/z) 352 (MH+); tR=3.47, (UV, ELSD) 96%, 99%. 1H NMR (500 MHz, DMSO-d6): 1.12 (m, 2H), 1.50 (m, 4H), 1.80 (m, 2H), 2.15 (m, 1H), 2.50 (d, 2H), 5.70 (broad s, 1H), 7.45 (s, 2H).

WORKUP

后处理

  1. temperatureby heating
  2. temperatureto reflux for 6 hours
  3. filtrationfiltered
  4. additiondiluted with water (250 ml)
  5. extractionAfter extraction
  6. concentrationthe combined organic phase was concentrated in vacuo