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3-Bromo-1-propanol → Ethyl 4-(2-(4-(3-hydroxypropyl)piperazin-1-yl)phenoxy)butanoate

HRID 887069
Notes
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Reaction equation

HRID 887069 reaction equation
[N:1]1([C:7]2[CH:21]=[CH:20][CH:19]=[CH:18][C:8]=2[O:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.Br[CH2:32][CH2:33][CH2:34][OH:35]>C(#N)C>[OH:35][CH2:34][CH2:33][CH2:32][N:4]1[CH2:3][CH2:2][N:1]([C:7]2[CH:21]=[CH:20][CH:19]=[CH:18][C:8]=2[O:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH2:6][CH2:5]1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 123083-Bromo-1-propanolHCID 81531DiisopropylethylamineHCID 57420183Ethyl 4-(2-(piperazin-1-yl)phenoxy)butanoate

Product 1

HCID 57420184Ethyl 4-(2-(4-(3-hydroxypropyl)piperazin-1-yl)phenoxy)butanoate

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
60 °C

Procedure

To a stirred solution of ethyl 4-(2-(piperazin-1-yl)phenoxy)butanoate 25 (0.48 g, 0.0016 mol) in 60 mL acetonitrile was added DIEA (0.56 mL, 0.0032 mol) followed by 3-bromo-1-propanol 26 (0.14 mL, 0.0016 mol) and the resulting mixture was stirred at 60° C. for 6 h. The progress of the reaction was monitored by thin layer chromatography (TLC). The reaction mixture was concentrated and the residue was diluted with DCM (50 mL). The reaction mixture was washed with water (50 mL×2), dried over magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography using 0-100% gradient of hexane and ethyl acetate to give the pure ethyl 4-(2-(4-(3-hydroxypropyl)piperazin-1-yl)phenoxy)butanoate 27. Brown oil, 0.39 g (63%). 1H NMR (400 MHz, CDCl3): δ 1.21 (t, J=7.2 Hz, 3H); 2.00 (quintet, J=7.2 Hz, 2H); 2.13 (quintet, J=7.2 Hz, 2H); 2.51 (t, J=7.2 Hz, 2H); 3.08 (broad s, 8H); 3.54 (t, J=6.4 Hz, 2H); 4.02 (t, J=6.4 Hz, 2H); 4.11 (q, J=7.2 Hz, 2H); 4.13-4.18 (m, 2H); 6.83-7.25 (m, 4H). MS (ESI): m/z=351.50 (M+H+).

Workup

  1. concentrationThe reaction mixture was concentrated
  2. additionthe residue was diluted with DCM (50 mL)
  3. washThe reaction mixture was washed with water (50 mL×2)
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography

Sources & evidence

ORD record
ord-59bdd5ab9ab24bd489ac1c5c38e90f0d
Source dataset
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08247420B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes