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Ammonia → trans-3-Octen-1-ol

HRID 9784
Notes
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Reaction equation

HRID 9784 reaction equation
[CH2:1]([OH:9])[CH2:2][C:3]#[C:4][CH2:5][CH2:6][CH2:7][CH3:8].CC(O)(C)C.N.[Li]>C1COCC1>[CH2:1]([OH:9])[CH2:2]/[CH:3]=[CH:4]/[CH2:5][CH2:6][CH2:7][CH3:8]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 222Ammonia2×HCID 6386tert-ButanolHCID 846943-Octyn-1-olHCID 3028194Lithium

Product 1

HCID 5364475trans-3-Octen-1-olYield 95.2%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

A solution of oct-3-yn-1-ol (2.52 g, 20.0 mmol), t-BuOH (5 g), THF (10 mL) and liquid NH3 was cooled to −36° C. Pieces of Lithium (0.34 g, 50 mmol) were introduced with vigorous stirrng and maintaining the temperature. After 2 h, NH3 was allowed to evaporate overnight. Saturated NH4Cl solution was added and the reaction mixture was extracted with hexane. The combined organic layers were washed with 1 M HCl, aqueous NaHCO3 and brine successively and dried. Evaporation of the solvent gave trans-oct-3-en-1-ol (2.44 g, 95%) as a pale yellow oil, which was used in the next step without further purification: 1H NMR (300 MHz, CDCl3) δ 5.54 (1H, m), 5.36 (1H, m), 3.66 (2H, t, J=6.3 Hz), 2.25 (2H, m), 2.02 (2H, m), 1.74 (1H, br s), 1.31 (4H, m), 0.88 (3H, t, J=7.2 Hz); 13C NMR (75 MHz, CDCl3) δ 134.27, 125.78, 62.22, 36.22, 32.59, 31.86, 22.47, 14.20.

Workup

  1. temperaturemaintaining the temperature
  2. customto evaporate overnight
  3. additionSaturated NH4Cl solution was added
  4. extractionthe reaction mixture was extracted with hexane
  5. washThe combined organic layers were washed with 1 M HCl, aqueous NaHCO3 and brine successively
  6. customdried
  7. customEvaporation of the solvent

Sources & evidence

ORD record
ord-2c2877b65fa545ce942d266c2a7f2895
Source dataset
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US07091357B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes