HRID373171

反应详情

EQUATION

反应方程式

HRID 373171 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

A slurry of 3-amino-5-dodecylisoxazole (2.20 g, 8.72 mmol) in acetonitrile (50 mL) was warmed until homogeneous. 2,6-Diisopropylphenyl-isocyanate (1.86 mL, 8.72 mmol) was then added in one portion and the resulting solution was heated under reflux for 6 hours. The resulting solution was cooled (25° C.), concentrated in vacuo, and chromatographed on silica (90:10 to 70;30 hexane:ethyl acetate). The product containing fractions were combined and concentrated to a solid which was washed with cold acetonitrile to yield 0.95 g (23.9%) of the title compound as a white solid, m.p. 101°-107° C.

WORKUP

后处理

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux for 6 hours
  3. concentrationconcentrated in vacuo
  4. customchromatographed on silica (90:10 to 70;30 hexane:ethyl acetate)
  5. additionThe product containing fractions
  6. concentrationconcentrated to a solid which
  7. washwas washed with cold acetonitrile