Water → HCID 9813323, compound

Participants

Reaction Conditions

Reaction Steps

1.5 g of the compound of Example 30 are dissolved in 10% aqueous sodium carbonate solution; the mixture is then extracted with ether, dried over sodium sulphate and concentrated to dryness. 1.17 ml of formol and 1.43 g of formic acid at 5° C. are then added to the residue obtained, followed by 0.15 ml of water. The mixture is heated at reflux for 5 hours, cooled to 50° C. and then made alkaline by the addition of 4N sodium hydroxide solution. Extraction with ether, followed by evaporation of the aqueous phase allows a residue to be obtained which is taken up in a mixture of 20 ml of ether and 3 ml of dioxane/4N hydrochloric acid. The mixture obtained is diluted with 50 ml of ether and stirred for 20 hours, and is then filtered and dried, allowing the expected product to be isolated.

Provenance & Evidence