Isopropanol hydrochloride → 1-Cyclopropylpiperazine dihydrochloride

HRID 1367621Notes

Reaction equation

HRID 1367621 reaction equation
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7](C(=O)C(F)(F)F)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.[ClH:16].CC(O)C>>[ClH:16].[ClH:16].[CH:1]1([N:4]2[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]2)[CH2:3][CH2:2]1

Participants

3

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-77994a8276e4457dbef6b385a07650ed
Source dataset
uspto-grants-2011_02
Patent number
US07893257B2

Reaction notes

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