反应详情

温度

50 °C

A mixture of 2-butoxy-2-oxoethanaminium chloride (573.5 g, 3.42 mol), triethylamine (415 g, 4.1 mol), and diethyl oxalate (1.0 kg, 6.8 mol) in ethanol (7 L) was heated at 50° C. for 3 hours. The product mixture was cooled and concentrated under vacuum. The residue was dissolved in methylene chloride and washed with two 4 L portions of water. The organic fraction was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residual oil was subjected to column chromatography on silica gel eluting with heptanes/ethyl acetate gradient. Collection and concentration of appropriate fractions provided the title material.

1. temperatureThe product mixture was cooled
2. concentrationconcentrated under vacuum
3. dissolutionThe residue was dissolved in methylene chloride
4. washwashed with two 4 L portions of water
5. dry with materialThe organic fraction was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. customCollection and concentration of appropriate fractions