Chloral Hydrate → HCID 86740595, compound

Participants

Reaction Conditions

Reaction Steps

A solution of 10.75 g (0.0345 mol) of N-methyl-4-phenyl-8-amino-isoquinoline hydrochloride in 22 ml of H2O was added to 6.23 g (0.0376 mol) of chloral hydrate in 86 ml of water. After 5 minutes, 42.5 g of Na2SO4 and a solution of 7.6 g (0.109 mol) of hydroxylamine hydrochloride in 36 ml of H2O were added. The reaction mixture was warmed to 106° C. (internal temperature) in the course of 40 minutes. After 2 minutes, the mixture was cooled rapidly to 18° C. with ice/H2O. 200 ml of methanol were added to the reaction mixture and a pH of 7.6 was established with 2N NaOH. The precipitate which had separated out was filtered off with suction and washed thoroughly with H2O. After drying, 9.7 g (90.2% of theory) of crude product of melting point 151.3° C. (Mettler FP 61) were obtained.

Provenance & Evidence