反应详情

Allyl bromide (2.91 g) was added dropwise to a stirred suspension of ethyl 2-(2-tritylaminothiazol-4-yl)-2-hydroxyiminoacetate (syn isomer, 10 g), N,N-dimethylformamide (100 ml) and potassium carbonate (4.54 g) under ice cooling over 5 minutes, and stirred at the same temperature for 4 hours. After adding water (200 ml) to the resultant solution, the solution was extracted with diethyl ether twice. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solution was concentrated in vacuo, and the residue was triturated with a solution of n-hexane and diethyl ether. The precipitates were collected by filtration to give ethyl 2-(2-tritylaminothiazol-4-yl)-2-allyloxyiminoacetate (syn isomer, 9.4 g), mp. 130° to 132° C.

1. extractionthe solution was extracted with diethyl ether twice
2. washThe extract was washed with a saturated aqueous solution of sodium chloride
3. dry with materialdried over magnesium sulfate
4. concentrationThe solution was concentrated in vacuo
5. customthe residue was triturated with a solution of n-hexane and diethyl ether
6. filtrationThe precipitates were collected by filtration