反应 #2200600

反应方程式

sodium methoxide

methyl 3-chloro-6-(chloromethyl)pyridine-2-carboxylate 1-oxide

→

methyl 3-chloro-6-(methoxymethyl)pyridine-2-carboxylate 1-oxide

溶剂

methanol

ethyl acetate

methanol

反应条件

后处理

1. 1
   洗涤washed with water
2. 2
   workup.ADDITIONTo the aqueous layer was added brine solution
3. 3
   萃取was extracted with ethyl acetate
4. 4
   干燥dried (MgSO4)
5. 5
   过滤filtered
6. 6
   浓缩concentrated to dryness

实验过程

A solution of methyl 3-chloro-6-(chloromethyl)pyridine-2-carboxylate 1-oxide (1.50 g, 6.35 mmol) in methanol (15 mL) was cooled to 0° C. A 25% solution of sodium methoxide in methanol (1.52 mL) was added and the mixture stirred at room temperature for 6 days. The reaction mixture was diluted with ethyl acetate and washed with water. To the aqueous layer was added brine solution and was extracted with ethyl acetate. The organic layers were combined, dried (MgSO4), filtered and concentrated to dryness to give crude methyl 3-chloro-6-(methoxymethyl)pyridine-2-carboxylate 1-oxide (1.14 g, 4.92 mmol) as a yellow oil; 1H NMR (CDCl3): δ 7.50 (d, 1H), 7.40 (d, 1H), 4.60 (s, 2H), 4.10 (s, 3H), 3.50 (s, 3H).

来源