HRID2287636

反应详情

EQUATION

反应方程式

HRID 2287636 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 1-chloro-3-[2-oxopyrrolidin-1-yl]propane (1 g, 6.2 mmol), 1-(3-chlorophenyl)piperazine (1.22 g, 6.2 mmol) anhydrous Na2CO3 (0.33 g, 3.1 mmol) and NaI (0.093 g, 0.6 mmol) in dry DMF (5 ml) was stirred at 70° C. for 14 hrs. The reaction mixture was cooled, poured on water (20 ml) and the separated residue was extracted with CHCl3 (2×25 ml). The extracts were dried over Na2SO4 and concentrated under reduced pressure to give 1-[4-(3-chlorophenyl)piperazin-1-yl]-3-[2-oxopyrrolidin-1-yl]propane as an oil which was purified by flash column chromatography over silica gel using chloroform as eluent, yield 1.50 g (75%) . IR (Neat): 3020, 2820, 1660, 1590, 1450, 1210, 730. 1H NMR (CDCl3): 1.30-2.60(m, 12H, 3', 4', 2, 1 & 2×N--CH2), 2.40-3.50(m, 8H, 5', 3 & 2×N--CH2), 6.40-7.20(m, 4H, ArH). MS: m/z 321 (M+) 323 (M+2).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. additionpoured on water (20 ml)
  3. extractionthe separated residue was extracted with CHCl3 (2×25 ml)
  4. dry with materialThe extracts were dried over Na2SO4
  5. concentrationconcentrated under reduced pressure