Potassium Carbonate → HCID 19767278, compound

A mixture of 5.8 g of N-methylformamide, 13.6 g of sodium hydroxide solution powder [sic], 5.8 g of potassium carbonate powder, 3.2 g of tetrabutylammonium bisulfate and 90 ml of dimethylpropyleneurea was stirred for 1 hour at room temperature. Thereafter, the resulting mixture was heated at 40° C. for 20 minutes and then to 70° C. At this temperature, a solution of 25 g of 11-bromoundecan-1-ol in 70 ml of dimethylpropyleneurea was added dropwise to the mixture. The resulting reaction mixture was then stirred for a further 12 hours at 70° C. and then poured onto 1.6 1 of water. The aqueous phase obtained was extracted with four times 180 ml of a solvent mixture of ether and ethyl acetate in a volume ratio of 1 1. The resulting organic phases were combined, and the combined organic phase was washed with three times 50 ml of water and then dried with sodium sulfate. After the sodium sulfate had been separated off and the organic solvent evaporated off, 20.5 g of N-methyl-N-(11-hydroxyundecyl)-formamide were obtained, which corresponded to a yield of 91%.

1. temperatureThereafter, the resulting mixture was heated at 40° C. for 20 minutes
2. customto 70° C
3. customThe resulting reaction mixture
4. stirringwas then stirred for a further 12 hours at 70° C.
5. customThe aqueous phase obtained
6. extractionwas extracted with four times 180 ml of a solvent mixture of ether and ethyl acetate in a volume ratio of 1 1
7. washthe combined organic phase was washed with three times 50 ml of water
8. dry with materialdried with sodium sulfate
9. customAfter the sodium sulfate had been separated off
10. customthe organic solvent evaporated off

ORD record

ord-3978da38fb0a4b7c84c3a778059223b6

Source dataset

uspto-grants-1993_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05204178