HRID517997
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 20 °C
PROCEDURE
实验过程
To a suspension of 5-bromo-3-(trifluoromethyl)pyridin-2-ol (500 mg) in 1,4-dioxane (10 ml), tert-butyl 2-hydroxyethyl(methyl)carbamate (475 mg) and triphenylphosphine (684 mg) were added. Then diisopropyl azodicarboxylate (556 mg) was dropwised and stirred at 20° C. for 1.5 h. The mixture was evaporated off the solvent and purified by Biotage SNAP cartridge KP-Sil column (50 g, heptane:ethyl acetate=1:0, 5:1, 4:1, 3:1 to 2:1) to give 630 mg yellow oil as tert-butyl 2-(5-bromo-3-(trifluoromethyl)pyridin-2-yloxy)ethyl(methyl)carbamate (76%).
WORKUP
后处理
- additionwere added
- customThe mixture was evaporated off the solvent
- custompurified by Biotage SNAP cartridge KP-Sil column (50 g, heptane:ethyl acetate=1:0, 5:1, 4:1, 3:1 to 2:1)