Potassium Hydroxide → HCID 14744528, compound
Reaction equation
[CH2:1]([O:3][C:4]1([O:16][CH2:17][CH3:18])[CH2:9][CH:8](C(OCC)=O)[C:7](=[O:15])[CH2:6][CH2:5]1)[CH3:2].[OH-].[K+]>>[CH2:17]([O:16][C:4]1([O:3][CH2:1][CH3:2])[CH2:9][CH2:8][C:7](=[O:15])[CH2:6][CH2:5]1)[CH3:18]Participants
3
Procedure
Into a flask are successively added 38.7 g of ethyl 5,5-diethoxy-2-oxocyclohexane carboxylate and 215 ml of a 10% potassium hydroxide solution. The mixture is refluxed for 16 hours, then cooled to room temperature. The organic phase is extracted twice with ether; the aqueous solution is salted out with potassium carbonate and an oily phase separates which is extracted with ether. The ethereal phases are united, dried over potassium carbonate and evaporated to dryness. The crude residue weighing 26.4 g is purified by distillation under reduced pressure. The yield amounts to 22.3 g of a liquid boiling at 110°-112° under 12 mm Hg -- nD22 = 1.449.
Workup
- customInto a flask are successively added
- temperatureThe mixture is refluxed for 16 hours
- extractionThe organic phase is extracted twice with ether
- extractionan oily phase separates which is extracted with ether
- dry with materialdried over potassium carbonate
- customevaporated to dryness
- distillationis purified by distillation under reduced pressure
Sources & evidence
- ORD record
- ord-32baa845a1ca4a8d97f480a62c8ec25c
- Source dataset
- uspto-grants-1978_04
- Patent number
- US04086355
Reaction notes
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