HRID233057

反应详情

EQUATION

反应方程式

HRID 233057 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-[1-phenylmethyl-2-pyrrolidinyl]phenol (1.0 g) in dry tetrahydrofuran (50 ml) was added methyl isocyanate (0.24 ml) followed by milled potassium carbonate (0.7 g) at ambient temperature, under nitrogen. The reaction mixture was stirred for 1 hr, filtered through a pad of celite, and the filter cake was washed with ethyl acetate. The combined filtrates were concentrated. The residue was purified by flash column chromatography (silica gel, dichloromethane/0-10% ethyl acetate). The appropriate fractions were collected and concentrated to give 0.8 g (70%) of product.

WORKUP

后处理

  1. filtrationfiltered through a pad of celite
  2. washthe filter cake was washed with ethyl acetate
  3. concentrationThe combined filtrates were concentrated
  4. customThe residue was purified by flash column chromatography (silica gel, dichloromethane/0-10% ethyl acetate)
  5. customThe appropriate fractions were collected
  6. concentrationconcentrated