Hydrochloric Acid → HCID 21190254, compound

HRID 1068786Notes

Reaction equation

HRID 1068786 reaction equation
[F:1][C:2]([F:29])([F:28])[S:3]([N:6]1[CH2:11][CH2:10][CH:9]([CH2:12][CH2:13][CH2:14][N:15]2[CH2:25][C:24]3[N:26]4[C:17](=[CH:18][N:19]=[C:20]4[CH:21]=[CH:22][CH:23]=3)[C:16]2=[O:27])[CH2:8][CH2:7]1)(=[O:5])=[O:4].[ClH:30]>C(O)C>[ClH:30].[F:29][C:2]([F:1])([F:28])[S:3]([N:6]1[CH2:7][CH2:8][CH:9]([CH2:12][CH2:13][CH2:14][N:15]2[CH2:25][C:24]3[N:26]4[C:17](=[CH:18][N:19]=[C:20]4[CH:21]=[CH:22][CH:23]=3)[C:16]2=[O:27])[CH2:10][CH2:11]1)(=[O:4])=[O:5]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21190248HCID 21190248, compound

Product 1

HCID 21190254HCID 21190254, compoundYield 81.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution prepared by dissolving 300 mg (0.70 mM) of 4,5-dihydro-4-[3-(1-trifluoromethanesulfonylpiperidin-4-yl)propan-1-yl]-3H-1,4,8b-triazaacenaphthylen-3-one in 10 ml of ethanol was added 0.12 ml (1.4 mM) of 12N hydrochloric acid at room temperature. After stirring, the solvent was distilled off under reduced pressure and 10 ml of 2-propanol was added to the residue. The precipitate that formed was recovered by filtration and rinsed with a small amount of ether to provide 265 mg (yield 81.1%) of the title compound as light-yellow solid.

Workup

  1. customTo a solution prepared
  2. distillationthe solvent was distilled off under reduced pressure and 10 ml of 2-propanol
  3. additionwas added to the residue
  4. customThe precipitate that formed
  5. filtrationwas recovered by filtration
  6. washrinsed with a small amount of ether

Sources & evidence

ORD record
ord-9600e671a9b64b13a4a847f123f18156
Source dataset
uspto-grants-2001_06
Patent number
US06251905B1

Reaction notes

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