反应 #2358494

反应方程式

Tert-butyl (3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]-2-oxo-azepane-1-carboxylate

hydrogen chloride

→

(3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]azepan-2-one

溶剂

dichloromethane

dichloromethane

反应条件

后处理

1. 1
   洗涤the reaction mixture was washed with sat. NaHCO3
2. 2
   萃取The aqueous layer was extracted once with dichloromethane
3. 3
   干燥dried over Na2SO4
4. 4
   其他the solvent was evaporated
5. 5
   其他to give the crude as a yellow solid
6. 6
   其他The residue was triturated in tertbutylmethylether
7. 7
   过滤the solid was filtered
8. 8
   其他dried

实验过程

Tert-butyl (3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]-2-oxo-azepane-1-carboxylate I-13b (0.55 g) was solved in dichloromethane (20 mL) and hydrogen chloride (2.0378 mL, 4M in dioxane) was added dropwise. After 30 min., dichloromethane was added and the reaction mixture was washed with sat. NaHCO3. The aqueous layer was extracted once with dichloromethane, the organic layers were combined, dried over Na2SO4 and the solvent was evaporated to give the crude as a yellow solid. The residue was triturated in tertbutylmethylether and the solid was filtered and dried to give (3E)-3-[(4-methyl-5-oxo-2H-furan-2-yl)oxymethylene]azepan-2-one Ia-13 (0.245 g, 63%) as a white solid. LCMS (Method D): 0.67 min; ES+238 (M+H+).

来源