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3-Methyl-2-buten-1-OL → 3,3-Dimethylallylglycidyl ether

HRID 47169
Notes
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Reaction equation

HRID 47169 reaction equation
[CH3:1][C:2]([CH3:6])=[CH:3][CH2:4][OH:5].[H-].[Na+].[CH2:9]([CH:11]1[O:13][CH2:12]1)Br>C1COCC1>[CH3:1][C:2]([CH3:6])=[CH:3][CH2:4][O:5][CH2:9][CH:11]1[O:13][CH2:12]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 111733-Methyl-2-buten-1-OLHCID 18430EpibromohydrinHCID 24758Sodium hydride

Product 1

HCID 155803333,3-Dimethylallylglycidyl ether

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of dimethylallyl alcohol (17.3 g, 20.5 mL, 0.2 mol) in dry THF (200 mL), sodium hydride (4.8 g, 0.2 mol) was added in portions and the mixture was stirred at room temperature for 1 hour. Epibromohydrin (27.4 g, 17.12 mL, 0.2 mol) was added to this reaction mixture dropwise and the mixture was stirred at room temperature for 24 hours. THF was removed on a rotary evaporator and the residue was taken up in ether and filtered. The ether solution was concentrated on a rotary evaporator and the brown oil obtained was distilled under vacuum to yield the title product. bp. 93-94° C./10 mm. Yield: 17.2 g (60.5%). 1H NMR (CDCl3) δ1.68 and 1.75 (s, 6H, CH3), 2.61 and 2.88 (dd,2H, oxirane CH2), 3.17 (m, 1H, oxirane CH), 3.38 and 3.7 (m, 2H, CH2OCH2CH), 4.05 (m, 2H, CH2OCH2CH), 5.35 .(m, 1H, >C═CH).

Workup

  1. stirringthe mixture was stirred at room temperature for 24 hours
  2. customTHF was removed on a rotary evaporator
  3. filtrationfiltered
  4. concentrationThe ether solution was concentrated on a rotary evaporator
  5. customthe brown oil obtained
  6. distillationwas distilled under vacuum

Sources & evidence

ORD record
ord-8a7ea803b1804dc29aa8ae7823c0926e
Source dataset
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06699458B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes