Isopropanol hydrochloride → 1-Cyclopropylpiperazine dihydrochloride

To 1-(4-cyclopropyl-piperazin-1-yl)-2,2,2-trifluoro-ethanone (444.4 mg, 2 mmol) was added a mixture of HCl/IPA (5-6N, 2 mL). Solids were observed to precipitate immediately after the HCl/IPA was added. The resulting suspension was stirred for 5 h. Heptane (2 mL) was then added to the reaction mixture, followed by addition of IPA (2 mL). The resulting suspension was stirred for 0.5 h at ambient temperature. The solids were filtered off using a medium glass sintered funnel with a filter paper on the top. The reaction flask was rinsed with IPA (3 mL) and the rinse was used to wash the solids. The solid was washed a second time with fresh IPA (2 mL). The solids were dried at ambient temperature and house vacuum to yield the title compound as a white crystalline solid.

1. customto precipitate immediately after the HCl/IPA
2. additionwas added
3. additionHeptane (2 mL) was then added to the reaction mixture
4. additionfollowed by addition of IPA (2 mL)
5. stirringThe resulting suspension was stirred for 0.5 h at ambient temperature
6. filtrationThe solids were filtered off
7. washThe reaction flask was rinsed with IPA (3 mL)
8. washto wash the solids
9. washThe solid was washed a second time with fresh IPA (2 mL)
10. customThe solids were dried at ambient temperature

ORD record

ord-b4af01ad411a4d70aa2fdf1221549630

Source dataset

uspto-grants-2014_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08680273B2