Hydrochloric Acid → HCID 69550587, compound

HRID 2214819Notes

Reaction equation

HRID 2214819 reaction equation
C(O)C.Cl.[Cl:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[CH:12]=[C:11]([S:16]([N:19]1[CH2:24][CH2:23][N:22]([CH2:25][C:26]3([NH:38][C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:31][CH2:30][N:29]([C:32]4[CH:37]=[CH:36][N:35]=[CH:34][CH:33]=4)[CH2:28][CH2:27]3)[C:21](=[O:44])[CH2:20]1)(=[O:18])=[O:17])[CH:10]=[CH:9]2.CCOCC>C(OCC)(=O)C>[ClH:5].[Cl:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[CH:12]=[C:11]([S:16]([N:19]1[CH2:24][CH2:23][N:22]([CH2:25][C:26]3([NH:38][C:39]([O:41][CH2:42][CH3:43])=[O:40])[CH2:27][CH2:28][N:29]([C:32]4[CH:37]=[CH:36][N:35]=[CH:34][CH:33]=4)[CH2:30][CH2:31]3)[C:21](=[O:44])[CH2:20]1)(=[O:18])=[O:17])[CH:10]=[CH:9]2

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 3283Diethyl EtherHCID 9829859HCID 9829859, compound

Product 1

HCID 69550587HCID 69550587, compoundYield 182.5%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

Ethanol (20 ml) and a 4N hydrochloric acid solution in ethyl acetate (2 ml) were added to 4-(6-chloronaphthalene-2-sulfonyl)-1-[4-ethoxycarbonylamino-1-(4-pyridyl)-4-piperidylmethyl]-2-piperazinone (1.3 g) obtained in Example 1, to dissolve the material. Subsequently, ethyl acetate (200 ml) and ether (200 ml) were added, the resulting precipitates were filtered off, and washed with ether to obtain the colorless amorphous title compound (1.26 g).

Workup

  1. dissolutionto dissolve the material
  2. customthe resulting precipitates
  3. filtrationwere filtered off
  4. washwashed with ether

Sources & evidence

ORD record
ord-8ed3ca507c624a9c83f49c8313322188
Source dataset
uspto-grants-2006_09
Patent number
US07109200B2

Reaction notes

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