Sodium Hydroxide → HCID 20370050, compound

HRID 596710Notes

Reaction equation

HRID 596710 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:18])([CH3:17])[CH2:9][C:10]#[C:11][C:12]([O:14]CC)=[O:13])=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]([CH3:18])([CH3:17])[CH:9]=[C:10]=[CH:11][C:12]([OH:14])=[O:13])=[CH:6][CH:7]=1

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 20370076HCID 20370076, compound

Product 1

HCID 20370050HCID 20370050, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

16 g of the product of Step B is dissolved in a minimum amount of ethanol and the solution added to 96 ml of 20% aqueous sodium hydroxide. Under a nitrogen atmosphere, the mixture is heated to 110° for 6 hours while permitting most of the ethanol to distill off. After cooling, the mixture is acidified to PH2 with conc. hydrochloric acid, the title product recovered by filtration, and refined by crystallization from petroleum ether, m.p. 64° - 67°.

Workup

  1. temperatureUnder a nitrogen atmosphere, the mixture is heated to 110° for 6 hours
  2. distillationto distill off
  3. temperatureAfter cooling
  4. filtrationthe title product recovered by filtration
  5. customrefined by crystallization from petroleum ether, m.p. 64° - 67°

Sources & evidence

ORD record
ord-411f27b7f5094db5b08fc2d3cf647803
Source dataset
uspto-grants-1977_03
Patent number
US04011339

Reaction notes

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