반응 #1519122

반응 방정식

TMS-triazole

Z-L-Pro-Cl

→

title compound

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

용매

sulfolane

sulfolane

brine

반응 조건

후처리

1. 1
   workup.WAITthe temperature is elevated to 140° C. for 3 hours
2. 2
   온도After the reaction mixture is cooled to rt
3. 3
   추출extracted with diethyl ether
4. 4
   세척The diethyl ether extracts are washed with brine
5. 5
   건조dried over anhydrous Na2SO4
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타The residue is purified by flash chromatography (DCM:acetone=9:1)

실험 절차

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.

출처