反应详情

A mixture of N-(ethoxycarbonylmethyl)-2-(4-hydroxymethylphenoxy)acetamide (3.96 g), triphenylphosphine (3.88 g), carbon tetrachloride (10 ml) and methylene chloride (20 ml) was heated at reflux for 1.5 hours. The reaction mixture was evaporated under reduced pressure, and ethyl acetate was added to the residue. After removal of the insolubles by filtration, the filtrate was chromatographed on silica gel column (eluent; ethyl acetate), and the desired fractions were collected and recrystallized from ethyl acetate/ether to give N-(ethoxycarbonylmethyl)-2-(4-chloromethylphenoxy)acetamide (2.8 g).

1. temperaturewas heated
2. temperatureat reflux for 1.5 hours
3. customThe reaction mixture was evaporated under reduced pressure, and ethyl acetate
4. additionwas added to the residue
5. customAfter removal of the insolubles
6. filtrationby filtration
7. customthe filtrate was chromatographed on silica gel column (eluent; ethyl acetate)
8. customthe desired fractions were collected
9. customrecrystallized from ethyl acetate/ether