反应 #4214

ord-b1182f573e4048b888b6653ec0ae28f6

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The solution was evaporated in vacuo
  2. 2
    其他to give a yellow oil
  3. 3
    其他The oil was chromatographed on silica gel (~300 g)
  4. 4
    洗涤eluting with 10% ethyl acetate/dichloromethane
  5. 5
    其他evaporated in vacuo

实验过程

N-(2-Oxo-1-imidazolidinyl)carbamic acid, 1,1-dimethylethyl ester (12.0 g, 0.06 mmol) was dissolved in dichloromethane (75 ml) containing pyridine (5.2 g, 0.066 mol). The solution was cooled to 0° C. and treated slowly with bromoacetyl bromide (13.3 g, 0.066 mol). The solution was evaporated in vacuo to give a yellow oil. The oil was chromatographed on silica gel (~300 g) eluting with 10% ethyl acetate/dichloromethane. The appropriate fractions were combined and evaporated in vacuo to give the title compound as a white solid, 16.7 g.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04723002uspto-grants-1988_02