Hydrochloric Acid → HCID 21994158, compound

HRID 1978512Notes

Reaction equation

HRID 1978512 reaction equation
[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:15][CH2:14][N:13]([C:16]([CH2:18][NH:19][C:20]([C:22]3[S:32][C:31]4[N:33]5[C:24](=[CH:25][N:26]=[C:27]5[CH:28]=[CH:29][CH:30]=4)[CH:23]=3)=[O:21])=[O:17])[CH2:12][CH2:11]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:34]>C(O)C>[ClH:34].[ClH:34].[C:1]1([CH2:7][CH2:8][CH2:9][N:10]2[CH2:11][CH2:12][N:13]([C:16]([CH2:18][NH:19][C:20]([C:22]3[S:32][C:31]4[N:33]5[C:24](=[CH:25][N:26]=[C:27]5[CH:28]=[CH:29][CH:30]=4)[CH:23]=3)=[O:21])=[O:17])[CH2:14][CH2:15]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21994063HCID 21994063, compound

Product 1

HCID 21994158HCID 21994158, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.306 g (2.83 mmol.) of N-[4-(3-phenylpropan-1-yl)piperazin-1-ylcarbonylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added, at room temperature, 1.5 ml (18 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes, which was concentrated under reduced pressure. To the resulting crystals were added ethanol and diethyl ether. The crystals were collected by filtration, which were washed with ether and diethyl ether to afford the object compound as orange crystals. The yield was 1.26 g (83%). m.p.189-196° C. (decomp.)

Workup

  1. concentrationwhich was concentrated under reduced pressure
  2. additionTo the resulting crystals were added ethanol and diethyl ether
  3. filtrationThe crystals were collected by filtration, which
  4. washwere washed with ether and diethyl ether

Sources & evidence

ORD record
ord-e15e2f64faad4721a3d04ad4b4f95a2a
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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