Hydroxide → HCID 12330037, compound

HRID 1196989Notes

Reaction equation

HRID 1196989 reaction equation
[Li].[OH-].O.[O:4]=[C:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][O:8][C:7]2[CH:16]=[CH:17][C:18]([CH2:20][C:21](OC)=[O:22])=[CH:19][C:6]1=2>O1CCCC1>[OH:4][CH:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][O:8][C:7]2[CH:16]=[CH:17][C:18]([CH2:20][CH2:21][OH:22])=[CH:19][C:6]1=2

Participants

6

Reactant 4

HCID 961HydroxideHCID 962WaterHCID 3028194LithiumHCID 10333952Methyl (11-oxo-6,11-dihydrodibenzo[b,e]oxepin-2-yl)acetate

Product 1

HCID 12330037HCID 12330037, compoundYield 97.5%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

In this process, 20 g of methyl 11-oxo-6,11-dihydrodibenz[b,e]oxepin-2-acetate is dissolved in 500 ml of tetrahydrofuran. To the solution is added 6.0 g of lithium alminium hydroxide and the mixture is stirred at room temperature for one hour. After decomposing an excess of the reagent by the addition of water to the solution, the mixture is filtered to remove an inorganic salts and the filtrate is concentrated to dryness under reduced pressure to obtain 17.7 g of the desired product as a white solid.

Workup

  1. filtrationthe mixture is filtered
  2. customto remove an inorganic salts
  3. concentrationthe filtrate is concentrated to dryness under reduced pressure

Sources & evidence

ORD record
ord-55e659176c684634bfaa07b5c8c6c3f9
Source dataset
uspto-grants-1992_05
Patent number
US05116863

Reaction notes

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