HRID2278960

反应详情

EQUATION

反应方程式

HRID 2278960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A 0° C. solution of 1-(tert-butyl)-3-(2-chloroethyl)urea (2.00 g, 11.19 mmol) in THF (20 mL) was treated with NaH (60% in mineral oil, 0.800 g, 33.3 mmol), stirred at RT for 1 h, then heated at 65° C. overnight. The mixture was cooled to RT, concentrated to dryness, treated with satd. NH4Cl, extracted with EtOAc (3×) and the combined organics were dried over Na2SO4 and concentrated to dryness to afford 1-(tert-butyl)imidazolidin-2-one (1.19 g, 75%). MS (ESI) m/z: 143.1 (M+H+).

WORKUP

后处理

  1. temperatureheated at 65° C. overnight
  2. temperatureThe mixture was cooled to RT
  3. concentrationconcentrated to dryness
  4. additiontreated with satd
  5. extractionNH4Cl, extracted with EtOAc (3×)
  6. dry with materialthe combined organics were dried over Na2SO4
  7. concentrationconcentrated to dryness