Potassium Carbonate → HCID 20083255, compound

HRID 1608937Notes

Reaction equation

HRID 1608937 reaction equation
[CH3:1][C:2]1([CH3:19])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]#[C:13][Si](C)(C)C)[CH:10]=2)[O:5][C:4](=[O:18])[CH2:3]1.C(=O)([O-])[O-].[K+].[K+]>CO>[CH3:1][C:2]1([CH3:19])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([C:12]#[CH:13])[CH:10]=2)[O:5][C:4](=[O:18])[CH2:3]1

Participants

4

Procedure

To a solution of 2.15 g (8.0 mmol) of 4,4-dimethyl-6-trimethylsilylethynyl-2-oxo-chroman in 25 ml of methanol was added, under nitrogen, 1.0 g of potassium carbonate. The reaction mixture was stirred at room temperature for 12 hours and the methanol was then removed under vacuum. The residue was extracted with methylene chloride (2×15 ml) and the combined organic layers were washed with dilute HCl, water, brine and dried (MgSO4). The solvent was removed in-vacuo and the residue purified by Kugelrohr distillation to give the title compound as a yellow oil.

Workup

  1. customthe methanol was then removed under vacuum
  2. extractionThe residue was extracted with methylene chloride (2×15 ml)
  3. washthe combined organic layers were washed with dilute HCl, water, brine
  4. dry with materialdried (MgSO4)
  5. customThe solvent was removed in-vacuo
  6. distillationthe residue purified by Kugelrohr distillation

Sources & evidence

ORD record
ord-9fb10a5123814a2194c2a5e94d78f487
Source dataset
uspto-grants-1995_03
Patent number
US05399561

Reaction notes

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