반응 #2358494

반응 방정식

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

용매

dichloromethane

dichloromethane

반응 조건

후처리

1. 1
   세척the reaction mixture was washed with sat. NaHCO3
2. 2
   추출The aqueous layer was extracted once with dichloromethane
3. 3
   건조dried over Na2SO4
4. 4
   기타the solvent was evaporated
5. 5
   기타to give the crude as a yellow solid
6. 6
   기타The residue was triturated in tertbutylmethylether
7. 7
   여과the solid was filtered
8. 8
   기타dried

실험 절차

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+).

출처