Water → HCID 13062099, compound

Participants

Reaction Steps

In a 500 ml three-necked flask of having a stirrer, a reflux condenser, a thermometer, and a dropping funnel there were placed 100 ml of anhydrous ethyl ether. When this had been cooled on an ice bath there were added 4 g of lithium hydride, and the contents of the flask were stirred for 15 minutes. There was then added very slowly a solution of 7.4 g of the product of Example 7 in 50 ml of anhydrous ethyl ether. The mixture was then heated under reflux for 2 hours and stirred for a further 15 hours at room temperature. It was then cooled on an ice bath and there were added dropwise 20 ml of water followed by 150 ml of dichloromethane. The mixture was then filtered over Celite, dried over sodium sulphate and concentrated by evaporation. There were obtained 7 g of an oil which could be crystallized to a product melting at 80° C.

Provenance & Evidence