反应详情

温度

0 °C

To an ice-cooled and stirred solution of 4.0 g (12 mmol) of the above prepared 2-[4-(tert-butoxycarbonylamino-methyl)-phenoxy]-2-methyl-propionic acid ethyl ester in 37 ml DMF was cooled (0° C.), and treated with 0.78 g (55% in oil, 18 mmol) of sodium hydride and, after 30 min, with 5.93 ml (95 mmol) of CH3I. The reaction was stirred at 0° C. to room temperature for 16 h. Subsequently, the solution was poured onto ice water, adjusted to pH 1 (with aqueous 1N HCl) and extracted with ether (two times). The organic layers were washed with water, dried (MgSO4), evaporated and purified by flash chromatography (SiO2, heptane/AcOEt=9:1) to finally give 3.68 g of the title compound as colorless oil.

1. stirringThe reaction was stirred at 0° C. to room temperature for 16 h
2. additionSubsequently, the solution was poured onto ice water
3. extractionextracted with ether (two times)
4. washThe organic layers were washed with water
5. dry with materialdried (MgSO4)
6. customevaporated
7. custompurified by flash chromatography (SiO2, heptane/AcOEt=9:1) to finally give 3.68 g of the title compound as colorless oil