反应 #1519122

反应方程式

TMS-triazole

Z-L-Pro-Cl

→

title compound

2-oxazol-2-yl-pyrrolidine-1-carboxylic acid benzyl ester

溶剂

sulfolane

sulfolane

brine

反应条件

后处理

1. 1
   workup.WAITthe temperature is elevated to 140° C. for 3 hours
2. 2
   温度After the reaction mixture is cooled to rt
3. 3
   萃取extracted with diethyl ether
4. 4
   洗涤The diethyl ether extracts are washed with brine
5. 5
   干燥dried over anhydrous Na2SO4
6. 6
   过滤filtered
7. 7
   其他evaporated
8. 8
   其他The residue is purified by flash chromatography (DCM:acetone=9:1)

实验过程

To a solution of TMS-triazole (14.17 g, 100.3 mmol, 1 equiv.) in sulfolane (290 mL) at rt under nitrogen, is added dropwise Z-L-Pro-Cl (26.85 g, 100.3 mmol, 1 equiv.) in sulfolane (70 mL). The resulting mixture is stirred at rt for 30 minutes, then the temperature is elevated to 140° C. for 3 hours. After the reaction mixture is cooled to rt, poured into excess brine and extracted with diethyl ether. The diethyl ether extracts are washed with brine, dried over anhydrous Na2SO4, filtered and evaporated. The residue is purified by flash chromatography (DCM:acetone=9:1) to give the title compound as a light yellow oil.

来源