Hydrochloric Acid → HCID 131716666, compound

HRID 1088756Notes

Reaction equation

HRID 1088756 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]([N:11]2[CH2:16][CH:15]=[C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:18]=3)[N:13]3[N:27]=[CH:28][C:29]([C:30]#[N:31])=[C:12]23)=[O:10])[CH2:4][CH2:3]1.[ClH:32]>C(OCC)(=O)C>[ClH:32].[ClH:32].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]([N:11]2[CH2:16][CH:15]=[C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([C:23]([F:25])([F:26])[F:24])[CH:18]=3)[N:13]3[N:27]=[CH:28][C:29]([C:30]#[N:31])=[C:12]23)=[O:10])[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 15100973HCID 15100973, compound

Product 1

HCID 131716666HCID 131716666, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

4,5-Dihydro-4-[(4-methyl-1-piperazinyl)acetyl]-7-[3-(trifluoromethyl)phenyl]pyrazolo[1,5-a]pyrimidine-3-carbonitrile was dissolved in hot ethyl acetate and treated with dilute ethanolic hydrochloric acid. Cooling produced a solid which was collected, washed with ether and dried. This solid was heated to boiling in 60 ml of acetonitrile, filtered and the filtrate diluted with 60 ml of ether and refrigerated. The solid was collected, washed with ether and dried, giving 600 mg of the desired product, mp 198° C. (eff.).

Workup

  1. temperatureCooling
  2. customproduced a solid which
  3. customwas collected
  4. washwashed with ether
  5. customdried
  6. temperatureThis solid was heated
  7. filtrationfiltered
  8. additionthe filtrate diluted with 60 ml of ether
  9. customThe solid was collected
  10. washwashed with ether
  11. customdried

Sources & evidence

ORD record
ord-e83117e6200a427082c443f2e062102a
Source dataset
uspto-grants-1990_10
Patent number
US04963553

Reaction notes

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