HRID1261301

反应详情

EQUATION

反应方程式

HRID 1261301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 231 (61 mg) in THF (2 mL) was added 2-phenylacetyl isothiocyanate (42 mg, 0.199 mmol). The reaction mixture was stirred for 3 hours, concentrated under reduced pressure and the residue was purified by column chromatography, eluent EtOAc/hexane (35:65), to produce yellow oil. Purification of this material by preparative HPLC (column C-18 Aquasil, gradient: 60% MeOH to 95% MeOH) afforded title compound 232a (25 mg, 26% yield) as a cream solid. Characterization of 232a is provided in the table 22.

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. customthe residue was purified by column chromatography, eluent EtOAc/hexane (35:65)
  3. customto produce yellow oil
  4. customPurification of this material by preparative HPLC (column C-18 Aquasil, gradient: 60% MeOH to 95% MeOH)