Formic Acid → HCID 21254473, compound

Temperature

0 °C

A total of 100 g (0.77 mol) of 1-(2-hydroxyethyl)piperazine was added dropwise to a stirred solution of 78.6 g (1.54 mol) of 90% formic acid at 0° C. To the resulting solution, 63.2 g (0.77 mol) of 37% formaldehyde was added dropwise. The solution was stirred at 0° C. for 15 minutes and heated on a stream bath for 3 hours. The solution was acidified with 150 ml of concentrated hydrochloric acid. The water was removed and the resulting residue dissolved in 200 ml of 25% NaOH, and extracted with chloroform. The organic layer was dried over MgSO4, filtered, and the solvent removed. The resulting residue was distilled to give 84.7 g (76%) (b.p. 96°-97° C./3 Torr) of the alcohol as a colorless liquid. The dihydrochloride salt was prepared by acidifying the free base to a pH of 1 and removing the water.

1. temperatureheated on a stream bath for 3 hours
2. customThe water was removed
3. dissolutionthe resulting residue dissolved in 200 ml of 25% NaOH
4. extractionextracted with chloroform
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. customthe solvent removed
8. distillationThe resulting residue was distilled

ORD record

ord-c15bb48a95284f47b9048d12fee9c626

Source dataset

uspto-grants-1993_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05227481