تفاعل #2358494

معادلة التفاعل

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

المذيبات

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   غسيلthe reaction mixture was washed with sat. NaHCO3
2. 2
   استخلاصThe aqueous layer was extracted once with dichloromethane
3. 3
   تجفيفdried over Na2SO4
4. 4
   أخرىthe solvent was evaporated
5. 5
   أخرىto give the crude as a yellow solid
6. 6
   أخرىThe residue was triturated in tertbutylmethylether
7. 7
   ترشيحthe solid was filtered
8. 8
   أخرىdried

الإجراء التجريبي

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+).

المصدر