Diisopropyl Ether → HCID 178507134, compound

Participants

Reaction Steps

The procedure used in Example 6 is followed. In a 211 ml autoclave, dissolve 1.85 g of 4-(5,7-difluoro-1H-benzimidazol-2-yl)-9H-fluoren-9-one oxime (Z,E), obtained in the previous stage, in a mixture of 70 ml of ethanol and 70 ml of tetrahydrofuran, add a spatula of Raney activated nickel and then subject to an initial hydrogen pressure of 1 bar and heat the autoclave at 60° for 6 hours. After cooling, the volume of hydrogen absorbed is 342 ml. After filtration of the catalyst, the filtrate is concentrated under reduced pressure and then taken up in a mixture of dichloromethane with a small amount of methanol and dried over magnesium sulphate, and the crude solid obtained is made into a paste with diisopropyl ether. In this way, we obtain 1.32 g of 4-(5,7-difluoro-1H-benzimidazol-2-yl)-9H-fluorene-9(R,S)-amine, in the form of a grey powder, which is used as it is in the following stage, with the following characteristics:

Provenance & Evidence