Hydrochloric Acid → HCID 21994055, compound

HRID 1978522Notes

Reaction equation

HRID 1978522 reaction equation
[O:1]=[C:2]1[CH2:7][N:6]([CH2:8][CH2:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:5][C:4](=[O:17])[N:3]1[CH2:18][CH2:19][NH:20][C:21]([C:23]1[S:33][C:32]2[N:34]3[C:25](=[CH:26][N:27]=[C:28]3[CH:29]=[CH:30][CH:31]=2)[CH:24]=1)=[O:22].[ClH:35]>C(O)C>[ClH:35].[ClH:35].[O:1]=[C:2]1[CH2:7][N:6]([CH2:8][CH2:9][CH2:10][C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:5][C:4](=[O:17])[N:3]1[CH2:18][CH2:19][NH:20][C:21]([C:23]1[S:33][C:32]2[N:34]3[C:25](=[CH:26][N:27]=[C:28]3[CH:29]=[CH:30][CH:31]=2)[CH:24]=1)=[O:22]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21994032HCID 21994032, compound

Product 1

HCID 21994055HCID 21994055, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

To a solution of 1.56 g (3.28 mmol.) of N-[2-(2,6-dioxo-4-(3-phenylpropan-1-yl)piperazin-1-yl)ethan-1-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (10 ml) was added, at room temperature, 2 ml (24 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes, which was concentrated under reduced pressure to leave crystals. To the crystals was added ethanol, which was subjected to filtration to collect the crystals. The crystals was washed with ethanol and diethyl ether to give the object compound as an orange crystalline product. The yield was 1.20 g (66%).

Workup

  1. concentrationwhich was concentrated under reduced pressure
  2. customto leave crystals
  3. filtrationwas subjected to filtration
  4. customto collect the crystals
  5. washThe crystals was washed with ethanol and diethyl ether
  6. customto give the object compound as an orange crystalline product

Sources & evidence

ORD record
ord-8b4fe9497f9d413c956bb5eb280c3a94
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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