HRID1481959
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
PROCEDURE
实验过程
To a solution of 2,6-dichloro-4-methylnicotinic acid (1.00 g, 4.85 mmol, 1 equiv) in tert-butyl acetate (24 mL) was added 70% perchloric acid (0.88 mL, 14.56 mmol, 3 equiv). After 1 h, reaction was diluted with DCM, washed cautiously with saturated aqueous sodium bicarbonate solution, dried (Na2SO4), and concentrated in vacuo to provide the product (1.21 g, 95%) as a pale yellow oil. 1H NMR (400 MHz, CDCl3) δ 7.15 (s, 1H), 2.37 (d, J=0.5 Hz, 3H), 1.62 (s, 9H); LCMS (ESI, M+1): 262.1.
WORKUP
后处理
- customreaction
- washwashed cautiously with saturated aqueous sodium bicarbonate solution
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo