Hydrochloric Acid → HCID 57066098, compound

Temperature

70 °C

4-(2-Tetrahydrofuroyl)piperazine (33.25 g, 180.7 mmol) (III) is dissolved in 165 mL water. 5N Hydrochloric acid (34.5 mL) is added and the suspension is heated to 70° C. with stirring. Sodium cyanate (13.1 g, 201.15 mmol) is added in small portion to the stirring solution and heating is continued for an additional 2 hours. The reaction mixture is concentrated under reduced pressure to yield a thick oil. Chloroform (100 mL) is added to the oil and the solution is heated to reflux. The hot solution is filtered and the filtrate is dried over Na2SO4. The dried solution is concentrated under reduced pressure to a thick yellow oil. Ether (50 mL) is added to the oil and white crystals precipitated out. The product is filtered, washed with ether (25 mL) and dried. The product is used without further purification (33.8 g, 82.3% yield).

1. temperatureheating
2. concentrationThe reaction mixture is concentrated under reduced pressure
3. customto yield a thick oil
4. temperaturethe solution is heated to reflux
5. filtrationThe hot solution is filtered
6. dry with materialthe filtrate is dried over Na2SO4
7. concentrationThe dried solution is concentrated under reduced pressure to a thick yellow oil
8. additionEther (50 mL) is added to the oil and white crystals
9. customprecipitated out
10. filtrationThe product is filtered
11. washwashed with ether (25 mL)
12. customdried
13. customThe product is used without further purification (33.8 g, 82.3% yield)

ORD record

ord-05dd20769f8d479ea34d3bb45da8865c

Source dataset

uspto-grants-1997_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05686612