Propylamine → HCID 86682303, compound

0.8 mol (65.8 ml) of n-propylamine were added dropwise within 0.5 h to 0.2 mol (25 ml) of ethyl 2-fluoroacetoacetat. The reaction mixture was heated and then held for 2 h at 60° C. Then it was evaporated to dryness, dissolved in 50 ml water and 60 ml ethanol and adjusted with 32% HCl to pH 3. It was again evaporated, dissolved in 300 ml ethyl acetate, filtered and again evaporated to dryness. 17 g of crude product was chromatographed over 800 g silica gel with ethyl acetate/hexane 1/1. After drying, 14 g of the title compound were obtained.

1. temperatureThe reaction mixture was heated
2. customThen it was evaporated to dryness
3. dissolutiondissolved in 50 ml water
4. customIt was again evaporated
5. dissolutiondissolved in 300 ml ethyl acetate
6. filtrationfiltered
7. customagain evaporated to dryness
8. custom17 g of crude product was chromatographed over 800 g silica gel with ethyl acetate/hexane 1/1
9. customAfter drying

ORD record

ord-eb119db03f7445929edcb5ad0a7f695d

Source dataset

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09394324B2