反应详情

Sodium hydride (1.05 eq) was slowly added at 0° C. to a solution of N-methyltrifluoro-acetamide (25 g) in DMF (140 mL). The mixture was stirred for 1 h at room temperature under nitrogen. Then, a solution of bromohexene (32.1 g) in DMF (25 mL) was added dropwise and the mixture was heated to 70° C. for 12 hours. The reaction mixture was poured on water (200 mL) and extracted with ether (4×50 mL), dried (MgSO4), filtered and evaporated to give 35 g of the target product 18 as a yellowish oil which was used without further purification in the next step.

1. temperaturethe mixture was heated to 70° C. for 12 hours
2. additionThe reaction mixture was poured on water (200 mL)
3. extractionextracted with ether (4×50 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated