Hydrochloric Acid → HCID 86658509, compound

In a round-bottom flask with a mounted reflux condenser and under nitrogen atmosphere, 40.0 g (0.48 mol) of 2-pyrrolidinone, 39.2 g (0.48 mol) of 36% aqueous formaldehyde, and 37.3 g (0.52 mol) of isobutyraldehyde were introduced while being stirred vigorously, mixed with 10.0 g of concentrated hydrochloric acid, whereby the mixture vigorously boiled up. After boiling had subsided, the mixture was heated to boiling in an oil bath (100° C.), and was kept boiling overnight. The clear, yellow reaction mixture was neutralized with 2N NaOH, extracted twice with ethyl acetate, the combined organic phases were washed with brine, dried on MgSO4, and completely concentrated by evaporation in a rotary evaporator. The dark-yellow oil that was obtained was fractionated in a vacuum. The product distilled at an overhead temperature of 71° C. and a pressure of 2·10−2 mbar. Yield: 14.8 g (19% of theory) of a colorless and almost odorless liquid.

1. temperatureIn a round-bottom flask with a mounted reflux condenser
2. temperaturethe mixture was heated
3. customto boiling in an oil bath
4. extractionextracted twice with ethyl acetate
5. washthe combined organic phases were washed with brine
6. customdried on MgSO4
7. concentrationcompletely concentrated by evaporation in a rotary evaporator
8. customThe dark-yellow oil that was obtained
9. distillationThe product distilled at an overhead temperature of 71° C.

ORD record

ord-57902c378f514103a0e88276efef7859

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08157950B2