反应详情

温度

0 °C

To a solution of tert-butyl 1-{[(2,4-dimethoxybenzyl)amino]methyl}cyclopentyl-carbamate (3.20 g, 8.78 mmol) in anhydrous THF (25 mL) was added Et3N (1.35 mL, 9.65 mmol). The solution was cooled to 0° C., treated with bromoacetyl bromide (0.84 mL, 9.65 mmol), and stirred for 3 h. The reaction was poured into ice water and extracted three times into Et2O. The combined organics were dried over Na2SO4, filtered, and concentrated in vacuo. The resulting crude material was subjected to column chromatography eluting with a gradient of 0-100% EtOAc/hexanes. Collection and concentration of the appropriate fractions afforded the product.

1. extractionextracted three times into Et2O
2. dry with materialThe combined organics were dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. washeluting with a gradient of 0-100% EtOAc/hexanes
6. customCollection and concentration of the appropriate fractions
7. customafforded the product