Acetic Acid → HCID 19890937, compound

Participants

Reaction Steps

To a stirred suspension of 10 g (0.025 mol) diselenosalicylic acid in 75 ml water is added 7.6 g (0.19 ml) sodium hydroxide, when the internal temperature rises slightly and the acid goes into solution. Then 20 g (0.189 mol) sodium carbonate and 11.6 g (0.067 mol) sodium dithionite are added with slight heating, followed by 2 h heating under reflux. After cooling to room temperature 9.8 g (0.06 mol) 2-picolyl chloride hydrochloride dissolved in 20 ml water are added dropwise and stirring is continued at room temperature for 14 h. Then 25% hydrochloric acid is added to adjust to pH 8 to 9 followed by acetic acid (98%) to pH 5-6. The precipitated white crude product is sucked off, washed neutral with water and recrystallized from 2-propanol (900 ml).

Provenance & Evidence