Lithium hydroxide, monohydrate → HCID 19077644, compound

HRID 1780826Notes

Reaction equation

HRID 1780826 reaction equation
O[Li].O.[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([O:13]CC)=[O:12])[CH:8]([C:16]([O:18]CC)=[O:17])[CH2:7]1)[CH3:5]>O.C1COCC1>[CH:4](=[C:6]1[CH2:10][CH:9]([C:11]([OH:13])=[O:12])[CH:8]([C:16]([OH:18])=[O:17])[CH2:7]1)[CH3:5]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 564797HCID 564797, compound

Product 1

HCID 19077644HCID 19077644, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent2×

Procedure

A solution of LiOH.H2O (5.1 g, 120 mmol) in 130 ml of water is added dropwise at 0° C. to a solution of the compound from Example VIII (13.1 g, 54.5 mmol) in 70 ml of THF. The solution is stirred at room temperature for 20 h, the THF is stripped off in vacuo and the residue is extracted once with 40 ml of ether. The aqueous phase is brought to pH 2 with 10% strength hydrochloric acid and extracted three times with 200 ml of ethyl acetate each time. The combined ethyl acetate phases are dried over Na2SO4 and the solvent is stripped off in vacuo.

Workup

  1. extractionthe residue is extracted once with 40 ml of ether
  2. extractionextracted three times with 200 ml of ethyl acetate each time
  3. dry with materialThe combined ethyl acetate phases are dried over Na2SO4

Sources & evidence

ORD record
ord-d5fa86465a0d4eb0a30caa40dc7443f1
Source dataset
uspto-grants-1997_05
Patent number
US05631291

Reaction notes

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