HRID660758

反应详情

EQUATION

反应方程式

HRID 660758 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a suspension of PS-isocyanate resin (100 mg) in THF is added TBAF (1M in THF, 0.5 mL) and the mixture is stirred at RT for 2 h. The resin is filtered off and the TBAF solution is added to a solution of 4-{3-benzyloxy-4-[1,1,4-trioxo-5-(2-trimethylsilanylethyl)-1,2,5-thiadiazolidin-2-yl]-phenyl}-3,3-dimethylbutyronitrile (25 mg, 0.047 mmol) in THF (5 mL). The mixture is stirred at RT for 18 h then is diluted with 1N HCl and extracted with EtOAc. The organic layer is washed with brine, dried over Na2SO4 and concentrated to give the title compound which is used directly in the next step.

WORKUP

后处理

  1. filtrationThe resin is filtered off
  2. stirringThe mixture is stirred at RT for 18 h
  3. extractionextracted with EtOAc
  4. washThe organic layer is washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated