反应详情

3,3,3-trifluoropropanoic acid (0.24 mmol) was dissolved in dry DCM (0.5 mL) in a 4 mL vial, added oxalyl chloride (0.24 mmol) and a catalytic amount of DMF. Stirred at rt for 1 h and added to a mixture of intermediate 4 (0.05 mmol) and Et3N (0.47 mmol) in dry DCM (0.5 mL). Stirred at rt for 16 h. Reaction mixture filtered through a syringe filter, added TFA (1 mL) and stirred at rt for 15 min. Reaction mixture added H2O (5 mL) and extracted with DCM (3×5 mL). The organic phase was dried (Na2SO4), filtered, concentrated in vacuo and redissolved in DMSO (1 mL). The pure compound was obtained by standard preparative HPLC purification.

1. stirringStirred at rt for 16 h
2. customReaction mixture
3. filtrationfiltered through a syringe
4. filtrationfilter
5. additionadded TFA (1 mL)
6. stirringstirred at rt for 15 min
7. customReaction mixture
8. extractionextracted with DCM (3×5 mL)
9. dry with materialThe organic phase was dried (Na2SO4)
10. filtrationfiltered
11. concentrationconcentrated in vacuo
12. dissolutionredissolved in DMSO (1 mL)
13. customThe pure compound was obtained by standard preparative HPLC purification