Lithium Hydroxide → HCID 23711565, compound

HRID 399040Notes

Reaction equation

HRID 399040 reaction equation
[C:1]([O:8]C)(=[O:7])[CH2:2][C:3]([O:5][CH3:6])=[O:4].[Li+:10].[OH-]>CO.O>[C:3]([O:5][CH3:6])(=[O:4])[CH2:2][C:1]([O-:8])=[O:7].[Li+:10]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 7943Dimethyl malonate

Product 1

HCID 23711565HCID 23711565, compoundYield 77.7%

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 962WaterSolvent

Procedure

A solution of 15.02 g of dimethyl malonate in 50 ml of MeOH was cooled to 15° C. and treated dropwise over a 2 h period with a solution of 2.4 g of LiOH in 20 ml of water. The mixture was stirred for 30 min after the addition was completed and then stripped of solvent under reduced pressure. The residue was taken up in 100 ml of hot MeOH, the solution cooled to room temperature and filtered. The filtrate was stripped of solvent to dryness. The residue was suspended in 100 ml of toluene and stripped further to remove the remaining water. The solution was cooled to room temperature and the precipitate collected by filtration to give 9.66 g (68%) of lithium mono methyl malonate. IR (cm-1): 1730, 1605, 1580.

Workup

  1. additionafter the addition
  2. filtrationfiltered
  3. customto remove the remaining water
  4. temperatureThe solution was cooled to room temperature
  5. filtrationthe precipitate collected by filtration

Sources & evidence

ORD record
ord-d312d01dbf4e4750ab040ffdfd9f2ed6
Source dataset
uspto-grants-1998_10
Patent number
US05817694

Reaction notes

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