تفاعل #361128

معادلة التفاعل

2-pentanone

glyoxylic acid monohydrate

phosphoric acid

→

4-keto-hept-2-enoic acid

المذيبات

ethyl ether dichloromethane

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas warmed at ca. 80° for 19 hours
2. 2
   غسيلwashed thoroughly with brine
3. 3
   أخرىEvaporation of the
4. 4
   تجفيفdried (magnesium sulphate) organic phase
5. 5
   أخرىgave a yellow viscous oil, which
6. 6
   أخرىon crystallization from ethyl ether/petroleum ether

الإجراء التجريبي

A mixture of 2-pentanone (17.1 g, 198 mmol), glyoxylic acid monohydrate (8.05 g, 88 mmol) and about 85% phosphoric acid (12 ml) was warmed at ca. 80° for 19 hours. On cooling to room temperature the mixture was diluted with ethyl ether/dichloromethane (100 ml, 1:1) and washed thoroughly with brine. Evaporation of the dried (magnesium sulphate) organic phase gave a yellow viscous oil, which on crystallization from ethyl ether/petroleum ether gave 4-keto-hept-2-enoic acid as colorless prisms: mp 100°-2°.

المصدر