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Methanol → Methyl 3,5-dihydroxy-6,8-decadienoate

HRID 1195397
Notes
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Reaction equation

HRID 1195397 reaction equation
[OH:1][CH:2]([CH2:8][C:9](=[O:15])[CH:10]=[CH:11][CH:12]=[CH:13][CH3:14])[CH2:3][C:4]([O:6][CH3:7])=[O:5].C(B(CC)CC)C.[BH4-].[Na+].CO>C1COCC1>[OH:1][CH:2]([CH2:8][CH:9]([OH:15])[CH:10]=[CH:11][CH:12]=[CH:13][CH3:14])[CH2:3][C:4]([O:6][CH3:7])=[O:5]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

6

Reactant 4

HCID 887MethanolHCID 7357TriethylboraneHCID 4311764Sodium borohydrideHCID 54125930Methyl 3-hydroxy-5-oxo-6,8-decadienoate

Product 1

HCID 53818818Methyl 3,5-dihydroxy-6,8-decadienoateYield 42.7%

Reagents, catalysts & solvents 1

HCID 8028
Tetrahydrofuran
Solvent

Conditions

Temperature
-78 °C

Procedure

To a cold (-15° C.) solution of methyl 3-hydroxy-5-oxo-6,8-decadienoate (18.5 g, 86.9 mmol) in THF (300 mL) was added triethylborane (1M in THF, 113 mL, 113 mmol) and the solution was stirred for 20 minutes. After the mixture was cooled to -78° C., NaBH4 (6 g, 159 mmol) and methanol (37.5 mL) were added. The solution was vigorously stirred for 30 minutes at -78° C. and at ambient temperature for 3 hours. The solvent was removed under reduced pressure and the residue was partitioned between 1N HCl and ethyl acetate. The organic layer was dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (diethyl ether:hexane/3:1) to afford 7.95 g (42.7%) of the title compound as a yellow oil.

Workup

  1. stirringThe solution was vigorously stirred for 30 minutes at -78° C. and at ambient temperature for 3 hours
  2. customThe solvent was removed under reduced pressure
  3. customthe residue was partitioned between 1N HCl and ethyl acetate
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue was purified by chromatography on silica gel (diethyl ether:hexane/3:1)

Sources & evidence

ORD record
ord-8ef127b07a3b44919c27e7434e8459c9
Source dataset
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05110940

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes