反应详情

A solution of 3.66 g (10 mmol) of the above prepared 2-{4-[(tert-butoxycarbonyl-methyl-amino)-methyl]-phenoxy}-2-methyl-propionic acid ethyl ester in 50 ml dichloromethane was treated at 0° C. with 3.98 ml TFA and stirred at room temperature for 16 h. The reaction was evaporated and treated with ice water, neutralized with NaHCO3 (pH=8) and extracted dichloromethane (two times). The organic phases were washed with water, dried (MgSO4), and evaporated to give 2.77 g of crude product. Purification by flash chromatography on SiO2 with CH2Cl2/MeOH (95:5) yielded 1.95 g of the title compound as brown-yellow oil.

1. customThe reaction was evaporated
2. additiontreated with ice water
3. extractionextracted dichloromethane (two times)
4. washThe organic phases were washed with water
5. dry with materialdried (MgSO4)
6. customevaporated
7. customto give 2.77 g of crude product
8. customPurification by flash chromatography on SiO2 with CH2Cl2/MeOH (95:5)