Hydrogen chloride-ethyl acetate → HCID 22318656, compound

HRID 497327Notes

Reaction equation

HRID 497327 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:30]2[CH2:35][CH2:34][N:33](C(OC(C)(C)C)=O)[CH2:32][CH2:31]2)[CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][CH2:19][C:20]3[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:23]=[CH:22][CH:21]=3)[CH2:12][CH2:11]2)=[CH:4][CH:3]=1.[ClH:43].C(OCC)(=O)C>C(OCC)(=O)C.CO>[ClH:43].[ClH:43].[ClH:43].[ClH:43].[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([N:30]2[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]2)[CH2:9][N:10]2[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][CH2:18][CH2:19][C:20]3[C:29]4[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:23]=[CH:22][CH:21]=3)[CH2:12][CH2:11]2)=[CH:4][CH:3]=1

Participants

5

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 22318670HCID 22318670, compound

Product 1

HCID 22318656HCID 22318656, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

0.62 g of 1-[2-(4-Fluorophenyl)-2-(4-t-butoxycarbonylpiperazino)ethyl]-4-(4-naphthalen-1-yl-butyl)piperazine was dissolved in a mixture of 3 ml of ethyl acetate and 3 ml of methanol, and 4 ml of 4M hydrogen chloride/ethyl acetate solution was added, followed by stirring at room temperature for 6 hours. The precipitated crystals were collected by filtration, and the crystals were washed with ethyl acetate to give 0.42 g of 1-[2-(4-fluorophenyl)-2-piperazinoethyl]-4-(4-naphthalen-1-yl-butyl)piperazine tetrahydrochloride as an oil.

Workup

  1. additionwas added
  2. filtrationThe precipitated crystals were collected by filtration
  3. washthe crystals were washed with ethyl acetate

Sources & evidence

ORD record
ord-561b37e9721244a597fd87527b54d7ef
Source dataset
uspto-grants-2005_09
Patent number
US06949552B2

Reaction notes

Loading…