反应详情

234.6 grams (2 moles) of methyl pivalate and 120 grams (2 moles) of sodium hydride (80 weight % suspension in white oil) were heated to 90° C. in 1500 ml of dry toluene. There were dropped in at this temperature after addition of 1 ml of methanol 233.3 grams (2 moles) of propionitrile within 2.5 hours. After the end of the development of hydrogen the suspension was extracted with a total of 1200 ml of water and after phase separation the aqueous phase was acidified with concentrated HCl to a pH of 2. The deposited oil was separated off, the water phase extracted with chloroform, the organic extracts combined, dried and concentrated. The residue was fractionated in a water jet vacuum. 2,4,4-trimethyl-3-oxopentanenitrile came over at 87° C./11 Torr in an amount of 226.1 grams (81.2% of theory).

1. additionThere were dropped in at this temperature
2. extractionAfter the end of the development of hydrogen the suspension was extracted with a total of 1200 ml of water
3. customafter phase separation the aqueous phase
4. customThe deposited oil was separated off
5. extractionthe water phase extracted with chloroform
6. customdried
7. concentrationconcentrated
8. customcame over at 87° C./11 Torr in an amount of 226.1 grams (81.2% of theory)