反応 #2358494

反応方程式

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

溶媒

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   洗浄the reaction mixture was washed with sat. NaHCO3
2. 2
   抽出The aqueous layer was extracted once with dichloromethane
3. 3
   乾燥dried over Na2SO4
4. 4
   その他the solvent was evaporated
5. 5
   その他to give the crude as a yellow solid
6. 6
   その他The residue was triturated in tertbutylmethylether
7. 7
   ろ過the solid was filtered
8. 8
   その他dried

実験手順

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+).

出典