Lithium Hydroxide → HCID 178506741, compound

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Reaction Conditions

Reaction Steps

Using the same apparatus as described in Example I, the flask is charged with 4000 parts of water and 840 parts of lithium hydroxide, monohydrate. The mixture is stirred until a solution is obtained. To the flask then is added 2670 parts of a 65% aqueous solution of p-phenolsulfonic acid, followed by 1100 parts of 3-chloro-1,2-propanediol. The resultant solution is heated at reflux (about 104° C.) for about 24 hours. The pH is adjusted to 8 by adding 25% aqueous lithium hydroxide solution. The solution is concentrated by heating under reduced pressure and then is cooled at 20°-25°C. C by placing the flask in a cold water-bath. Solid precipitates. The solid is isolated by suction filtration and washed three times with 1000 parts of isopropanol. The solid then is reslurried in 9:1 isopropanol-water, filtered, and washed several times with 9:1 isopropanol-water. The isolated product is reslurried, filtered, and washed a second time. The dried product, 3-(4-lithiosulfophenoxy)-1,2-propanediol, is obtained in a yield of 980 parts and with a purity of 99%, based upon adjacent hydroxyl group analysis; the product contains 0.05% chloride. Elemental analysis of the product gives the following results:

Provenance & Evidence