Ammonia → HCID 86682299, compound

Temperature

90 °C

0.4 mol (63.7 ml) 3-oxo-heptanoic acid methylester and 400 ml 7 N ammonia solution was stirred for three hours at 100° C. in a pressure reactor. 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 4 hours and then again concentrated to dryness in the rotavap, taken up in 600 ml dichloromethane and washed 3 times with 100 ml water. The organic phase was distilled off and the raw product recrystallized from 100 ml toluene. The product was filtrated off and dried in a vacuum drying cabinet at 50° C. 3.5 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. washwashed 3 times with 100 ml water
5. distillationThe organic phase was distilled off
6. customthe raw product recrystallized from 100 ml toluene
7. filtrationThe product was filtrated off
8. customdried in a vacuum
9. customdrying cabinet at 50° C

ORD record

ord-80f432a98b764459888eefdcb2333ded

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394324B2