Methylamine → HCID 86682300, compound

Temperature

90 °C

0.378 mol (60.2 ml) 3-oxo-heptanoic acid methylester, 400 ml 33% methylamine solution in ethanol and 40 ml water were stirred for 48 hours at 80° C. in a round-bottomed flask with a reflux condenser. After cooling off, the solvents were distilled off on a rotavap, the raw products were taken up in 200 ml water and 40 ml ethanol and set to about pH 3 with 40 ml 32% HCl. The reaction mixture was heated to 90° C. for 24 hours and then again concentrated to dryness in the rotavap. The raw product heated with 150 ml to reflux, filtrated hot and the filtrate was left to cool off. The product was filtrated off and dried in a vacuum drying cabinet at 50° C. 5.9 g of the title compound was obtained.

1. temperatureAfter cooling off
2. distillationthe solvents were distilled off on a rotavap
3. concentrationagain concentrated to dryness in the rotavap
4. temperatureThe raw product heated with 150 ml
5. temperatureto reflux
6. filtrationfiltrated hot
7. waitthe filtrate was left
8. temperatureto cool off
9. filtrationThe product was filtrated off
10. customdried in a vacuum
11. customdrying cabinet at 50° C

ORD record

ord-1389850d2fea4906b6700c126b051338

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394324B2