Hydrochloric Acid → HCID 21994057, compound

HRID 1978488Notes

Reaction equation

HRID 1978488 reaction equation
[CH2:1]([CH:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:36]=[CH:35][C:18]([CH2:19][NH:20][C:21]([C:23]3[S:33][C:32]4[N:34]5[C:25](=[CH:26][N:27]=[C:28]5[CH:29]=[CH:30][CH:31]=4)[CH:24]=3)=[O:22])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:37]>C(O)C>[ClH:37].[ClH:37].[CH2:1]([CH:8]1[CH2:9][CH2:10][N:11]([CH2:14][C:15]2[CH:36]=[CH:35][C:18]([CH2:19][NH:20][C:21]([C:23]3[S:33][C:32]4[N:34]5[C:25](=[CH:26][N:27]=[C:28]5[CH:29]=[CH:30][CH:31]=4)[CH:24]=3)=[O:22])=[CH:17][CH:16]=2)[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21994004HCID 21994004, compound

Product 1

HCID 21994057HCID 21994057, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 1.73 g (3.50 mM) of N-[4-(4-benzylpiperidin-1-ylmethyl)benzyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (12 ml) was added 1 ml (12 mM) of 12N-hydrochloric acid at room temperature, and the mixture was stirred for several minutes (crystals separated out). This reaction mixture was concentrated under reduced pressure and ethanol and diethyl ether were added to the residue. The crystal crop was then harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals.

Workup

  1. custom(crystals separated out)
  2. concentrationThis reaction mixture was concentrated under reduced pressure and ethanol and diethyl ether
  3. additionwere added to the residue
  4. filtrationThe crystal crop was then harvested by filtration
  5. washrinsed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-113aab53ef064eff8c766194c0d2e776
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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