Lithium hydroxide, monohydrate → HCID 54712960, compound

HRID 1357193Notes

Reaction equation

HRID 1357193 reaction equation
O[Li].O.C([O:7][C:8]1[C:13]([CH3:14])=[C:12]([C:15]2[O:16][C:17]3[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=3[CH:19]=2)[O:11][C:10](=[O:24])[C:9]=1[CH3:25])(=O)C>CO>[O:16]1[C:17]2[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=2[CH:19]=[C:15]1[C:12]1[O:11][C:10](=[O:24])[C:9]([CH3:25])=[C:8]([OH:7])[C:13]=1[CH3:14]

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 15462824HCID 15462824, compound

Product 1

HCID 54712960HCID 54712960, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

An aqueous solution (30 ml) of LiOH-hydrate (465 mg) was added to a solution of 4-acetyloxy-6-(benzofuran-2-yl)-3,5-dimethyl-2H-pyran-2-one (3.00 g) in MeOH (100 ml) at 0° C., and after stirring at room temperature for 2 hours, the MeOH was distilled off under reduced pressure. The residue was rinsed with Et2O, and then a KHSO4 aqueous solution was added at 0° C. for adjustment to pH 2.0. The precipitated crystals were filtered off and thoroughly rinsed with water and Et2O in that order and then dried to obtain 6-(benzofuran-2-yl)-3,5-dimethyl-4-hydroxy-2H-pyran-2-one.

Workup

  1. distillationthe MeOH was distilled off under reduced pressure
  2. washThe residue was rinsed with Et2O
  3. additiona KHSO4 aqueous solution was added at 0° C. for adjustment to pH 2.0
  4. filtrationThe precipitated crystals were filtered off
  5. washthoroughly rinsed with water and Et2O in that order
  6. customdried

Sources & evidence

ORD record
ord-e269513692f44cfbaabef791ecf1a994
Source dataset
uspto-grants-2003_07
Patent number
US06589984B1

Reaction notes

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