Hydrogen chloride-ethyl acetate → HCID 69551091, compound

HRID 2214823Notes

Reaction equation

HRID 2214823 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([NH:34][C:35](=[O:39])[O:36][CH2:37][CH3:38])[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)[CH2:24][CH2:23]3)[C:17](=[O:40])[CH2:16]1)(=[O:14])=[O:13])[CH:6]=[CH:5]2.[ClH:41].C(OCC)(=O)C>C(O)C>[ClH:41].[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:20][CH2:19][N:18]([CH2:21][C:22]3([NH:34][C:35](=[O:39])[O:36][CH2:37][CH3:38])[CH2:23][CH2:24][N:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)[CH2:26][CH2:27]3)[C:17](=[O:40])[CH2:16]1)(=[O:14])=[O:13])[CH:6]=[CH:5]2

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 69551092HCID 69551092, compound

Product 1

HCID 69551091HCID 69551091, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ethyl 4-[[4-[(6-bromo-2-naphthyl)sulfonyl]-2-oxo-1-piperazinyl]methyl]-1-(4-pyridinyl)-4-piperidinylcarbamate (2.0 g) obtained in Example 17 was suspended in ethanol (20 ml), and 4N hydrochloric acid/ethyl acetate (1.2 ml) was added thereto at room temperature, followed by concentration under reduced pressure. The residue was dissolved in ethanol (8 ml), and ethyl acetate (50 ml) and diethyl ether (50 ml) were added. The resulting powders were collected to obtain the title compound (1.82 g) as colorless powders.

Workup

  1. concentrationat room temperature, followed by concentration under reduced pressure
  2. dissolutionThe residue was dissolved in ethanol (8 ml)
  3. additionethyl acetate (50 ml) and diethyl ether (50 ml) were added
  4. customThe resulting powders were collected

Sources & evidence

ORD record
ord-442e62e9c11f484db3420b075ad93dfb
Source dataset
uspto-grants-2006_09
Patent number
US07109200B2

Reaction notes

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