Hydrochloric Acid → Ethyl butyrimidate hydrochloride

Temperature

-20 °C

Butyronitrile (85 ml, 839 mmol) is dissolved in absolute ethanol (65 ml, 961 mmol) and cooled to 0° C. to 5° C. While cooling further, gaseous hydrogen chloride (about 40 g, about 1.1 mol, differential weighing of the pressure cylinder) is passed into the solution. The reaction mixture is left at about 4° C. for 96 hours and then, while stirring, 260 ml of diisopropyl ether are added, and the mixture is cooled to −20° C. and filtered with suction at 0° C. through a sintered funnel. The crystals are rapidly (the product is hygroscopic) washed twice with 50 ml of cold diisopropyl ether each time and stored, sealed air-tight, in a refrigerator.

1. temperaturecooled to 0° C. to 5° C
2. temperatureWhile cooling further
3. filtrationfiltered with suction at 0° C. through a sintered funnel
4. washwashed twice with 50 ml of cold diisopropyl ether each time
5. customsealed air-tight, in a refrigerator

ORD record

ord-2c90d4ad0a1b43caaac676c6f6439741

Source dataset

uspto-grants-2006_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07022847B2