Ammonia → HCID 178446961, compound

Participants

Reaction Steps

To a solution of sodium metal (0.7 g) in n-propyl alcohol (200 mL) was fed gaseous ammonia at a flow rate of 120 mL/min. at room temperature for 1 hour. Then, 22.8 g of 4-(2-aminophenylthio)-5-chloro-3,6-diisopentoxyphthalonitrile was added and the mixture was stirred at 50~60° C. for 20 hours. After cooling, n-propyl alcohol was distilled off and the residue was dissolved in 200 mL of toluene under warming at 30~40° C. Then, 500 mL of water was added and the mixture was stirred for dispersing and allowed to stand for phase separation. The above procedure was repeated 4 times to wash the toluene solution. The toluene was then distilled off and 200 mL of n-heptane was added. The mixture was stirred at 60~65° C. for 30 minutes and then cooled to room temperature. The resulting crystals were collected and dried to provide 20.3 g (yield 85.8%) of 5-(2-aminophenylthio)-6-chloro-1,3-diimino-4,7-diisopentoxyisoindoline. ##STR9##

Provenance & Evidence