HRID1591965

反应详情

EQUATION

反应方程式

HRID 1591965 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

The title C compound, 2-(4-methoxybenzyl)-1,1-dioxo-5-pyridin-4-ylmethyl-1,2,5-thiadiazolidin-3-one (73 mg, 0.21 mmol) in a mixture of TFA (4.75 mL) and triethylsilane (0.25 mL) in a 20 mL scintillation vial with polyseal cap is heated in an 80° C. oil bath for 16 h. The reaction solvents are removed by overnight evaporation on a Savant SpeedVac system. This gives a white solid which is dissolved in water, filtered through a 0.45 micron PTFE filter disc, and water is removed by lyophilization to give 1,1-dioxo-5-pyridin-4-ylmethyl-1,2,5-thiadiazolidin-3-one TFA salt as an amorphous white solid: [M+1]+=228.

WORKUP

后处理

  1. customcap
  2. customThe reaction solvents are removed by overnight
  3. customevaporation on a Savant SpeedVac system
  4. customThis gives a white solid which
  5. filtrationfiltered through a 0.45 micron PTFE
  6. filtrationfilter disc, and water
  7. customis removed by lyophilization