Hydrochloric Acid → HCID 70243697, compound

HRID 1978516Notes

Reaction equation

HRID 1978516 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][CH:10]([C:26]([NH:28][CH:29]2[CH2:34][CH2:33][NH:32][CH2:31][CH2:30]2)=[O:27])[NH:11][C:12]([C:14]2[S:24][C:23]3[N:25]4[C:16](=[CH:17][N:18]=[C:19]4[CH:20]=[CH:21][CH:22]=3)[CH:15]=2)=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:35]>C(O)C>[ClH:35].[ClH:35].[C:1]1([CH2:7][CH2:8][CH2:9][CH:10]([C:26]([NH:28][CH:29]2[CH2:30][CH2:31][NH:32][CH2:33][CH2:34]2)=[O:27])[NH:11][C:12]([C:14]2[S:24][C:23]3[N:25]4[C:16](=[CH:17][N:18]=[C:19]4[CH:20]=[CH:21][CH:22]=3)[CH:15]=2)=[O:13])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 70243698HCID 70243698, compound

Product 1

HCID 70243697HCID 70243697, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 303.2 mg (0.64 mmol.) of N-[1-(3-phenylpropan-1-yl)piperidin-4-ylaminocarbonylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (5 ml) was added, at room temperature, 0.5 ml (6.0 mmol.) of 12N hydrochloric acid. The mixture was stirred for one hour. The mixture was concentrated under reduced pressure. To the concentrate were added ethanol and diethyl ether. The resulting crystals were collected by filtration and washed with ethanol and diethyl ether to afford the object compound as orange crystals. The yield was 257.5 mg (73%).

Workup

  1. concentrationThe mixture was concentrated under reduced pressure
  2. additionTo the concentrate were added ethanol and diethyl ether
  3. filtrationThe resulting crystals were collected by filtration
  4. washwashed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-8a0d0cc7cc9b4bdd95568a9e45b8dfcd
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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