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O-(prop-2-yn-1-yl)hydroxylamine → HCID 136127200, compound

HRID 2164370
Notes
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Reaction equation

HRID 2164370 reaction equation
[C:1]([C:6]1[C:7](=[O:23])[CH2:8][CH:9]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([S:21][CH3:22])=[O:20])=[CH:15][CH:14]=2)[CH2:10][C:11]=1[OH:12])(=O)[CH2:2][CH2:3][CH3:4].[CH2:24]([O:27][NH2:28])[C:25]#[CH:26]>O1CCCC1>[OH:12][C:11]1[CH2:10][CH:9]([C:13]2[CH:14]=[CH:15][C:16]([C:19]([S:21][CH3:22])=[O:20])=[CH:17][CH:18]=2)[CH2:8][C:7](=[O:23])[C:6]=1[C:1](=[N:28][O:27][CH2:24][C:25]#[CH:26])[CH2:2][CH2:3][CH3:4]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 10749134O-(prop-2-yn-1-yl)hydroxylamineHCID 178450326HCID 178450326, compound

Product 1

HCID 136127200HCID 136127200, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Into 20 ml of tetrahydrofuran was dissolved 2 g of 2-butyryl-3-hydroxy-5-[4-(methylthio)carbonylphenyl]-2-cyclohexen-1-one and to the solution was added 0.7 g of propargyloxyamine. The mixture was kept for 15 hours at room temperature and the solvent was distilled off from it under reduced pressure. Then, the residue was recrystallized with mixture solvent of benzene-ligroin and 1.6 g of colorless desired crystals having a melting point of 95°-96° C. were obtained.

Workup

  1. distillationthe solvent was distilled off from it under reduced pressure
  2. customThen, the residue was recrystallized with mixture solvent of benzene-ligroin and 1.6 g of colorless desired crystals
  3. customwere obtained

Sources & evidence

ORD record
ord-39b9085a24044f8ebb956410d1d920ea
Source dataset
uspto-grants-1985_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US04504305

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes