HRID2218509

反应详情

EQUATION

反应方程式

HRID 2218509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(3-aminopropyl)-2-pyrrolidinone (560 μL, 4 mmol) and benzoyl isothiocyanate (536 μL, 4 mmol) was dissolved in chloroform (3 mL), stirred at room temperature for 30 min, then concentrated in vacuo. The resulting residue was dissolved in concentrated HCl (3 mL), heated at 95° C. for 2 h, then concentrated in vacuo. The resulting residue was dissolved in water and washed with dichloromethane (2×30 mL), then basified with 2 M NaOH and extracted with dichloromethane (2×30 mL). The combined extracts were dried over MgSO4 and concentrated to provide 1-(3-(2-oxopyrrolidin-1-yl)propyl)thiourea (638 mg) as a pale yellow oil.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe resulting residue was dissolved in concentrated HCl (3 mL)
  3. temperatureheated at 95° C. for 2 h
  4. concentrationconcentrated in vacuo
  5. dissolutionThe resulting residue was dissolved in water
  6. washwashed with dichloromethane (2×30 mL)
  7. extractionextracted with dichloromethane (2×30 mL)
  8. dry with materialThe combined extracts were dried over MgSO4
  9. concentrationconcentrated