Hydrochloric Acid → HCID 86658511, compound

In a round-bottom flask with a mounted reflux condenser and under nitrogen atmosphere, 59.7 g (1.00 mol) of N-methylformamide, 84.3 g (1.00 mol) of 36% aqueous formaldehyde, and 78.6 g (1.10 mol) of isobutyraldehyde were introduced while being stirred vigorously, mixed with 18.2 g of concentrated hydrochloric acid (slight exothermicity). After that, the mixture was heated to boiling in an oil bath (100° C.) and was kept boiling overnight. The clear, yellow reaction mixture was cooled to room temperature, 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 63° C. and a pressure of 4·10−2 mbar. Yield: 20.2 g (14% of theory) of colorless, slightly pungent-smelling liquid.

1. temperatureIn a round-bottom flask with a mounted reflux condenser
2. temperatureAfter that, the 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 63° C.

ORD record

ord-b7fafb67df0746d8ab50fd7a2c6f35de

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08157950B2