Ethylene Glycol → 2-Phenyl-ethenesulfonic acid [5-(4-chloro-phenyl)-6-(2-hydroxy-ethoxy)-pyrimidin-4-yl]-amide

Participants

Reaction Conditions

Reaction Steps

6.20 g of 2-phenyl-ethenesulfonic acid [6-chloro-5-(4-chloro-phenyl)-pyrimidin-4-yl]-amide was added to a solution of 7.65 g of potassium-tert.-butylate in 100 ml of ethylene glycol. The resulting solution was heated to 110° C. and stirred for 17 h. The ethylene glycol was evaporated under high vacuum and the remaining residue was treated with 250 ml of cold water. The suspension was acidified by adding 10 g of citric acid monohydrate and stirred at 0° C. for 15 min. The precipitate was collected, washed with water and dried to give 6.71 g of 2-phenyl-ethenesulfonic acid [5-(4-chloro-phenyl)-6-(2-hydroxy-ethoxy)-pyrimidin-4-yl]-amide as a white powder. LC-MS: tR=4.55 min, [M+H]+=432.00 (ES+), [M−H]−=429.98 (ES−).

Provenance & Evidence