反应详情

温度

100 °C

A mixture of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (1.1 g, 4.5 mmol, prepared as described in WO 2007/090748), N-bromosuccinimide (2.86 g, 16.1 mmol) and benzoyl peroxide (0.21 g, 0.9 mmol) in carbon tetrachloride (9 mL) was heated in a sealed vessel to 100° C. overnight. The mixture was diluted with dichloromethane (DCM), filtered and the solvent was removed in vacuo. Purification via preparative HPLC-MS (C18 eluting with a gradient of MeCN/H2O containing 0.15% NH4OH) afforded the product, which on removal of solvent, was an oil.

1. filtrationfiltered
2. customthe solvent was removed in vacuo
3. customPurification via preparative HPLC-MS (C18
4. washeluting with a gradient of MeCN/H2O containing 0.15% NH4OH)
5. customafforded the product, which
6. customon removal of solvent