HRID892803

反应详情

EQUATION

反应方程式

HRID 892803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium hexamethyl disilazide (0.6 mL, 1.0M in hexanes) was added at 0° C. under nitrogen to a solution of N-(3-benzoylphenyl) 2-(3-pyridinyl)-3-tert-butoxycarbonyl-4-thiazolidinecarboxamide prepared as described in example 2 (202 mg, 0.41 mmol), in dry THF (4 mL, 0.1 mL). The mixture was stirred for 20 min then methyl iodide (25 μL) was added and the mixture stirred for an additional 8 hours. The reaction mixture was partioned between ethyl acetate and saturated sodium bicarbonate solution. The organic phase was dried over magnesium sulfated and the solvent removed in vacuo. The residue was purified by flash chromatography eluting with hexanes:ethyl acetate (12:3) to yield the desired product (0.53 g, 45%).

WORKUP

后处理

  1. customprepared
  2. stirringthe mixture stirred for an additional 8 hours
  3. dry with materialThe organic phase was dried over magnesium
  4. customthe solvent removed in vacuo
  5. customThe residue was purified by flash chromatography
  6. washeluting with hexanes:ethyl acetate (12:3)