Ammonia → HCID 19782853, compound

Participants

Reaction Conditions

Reaction Steps

A typical run consisted of charging the reactor with 35 grams of 2,2-bis(3-nitro-4-hydroxyphenyl)propane, 20 grams of ammonium chloride, 40 ml of water and a stirring bar. The vessel was capped and placed in a -70° C. freezer overnight to freeze the contents. Ammonia was condensed into a 100 ml flask until 63 ml had been collected. The ammonia was added to the reaction vessel and the vessel bolted shut. A variable transformer and heating tape were used to heat the contents to 140° C. for 30 hours and a stirring plate was used to keep the reaction well mixed. The vessel was then allowed to cool to room temperature and vented to release the excess ammonia. The contents were slurried with 500 ml of 1 molar sodium hydroxide solution to dissolve the unreacted starting materials. The slurry was filtered, washed with distilled water, and dried. Recrystallization from toluene and vacuum sublimation gave 32.5 grams (93%) of orange 2,2-bis(3-nitro-4-aminophenyl)propane melting at 207°-210° C. Several runs of the amination reaction were completed to produce enough material for the reduction step. Analysis calculated for C15H16N4O4 : C, 56.96%; H, 5.10%; N, 17.71%; 0, 20.23%. Found: C, 57.06%; H, 5.23%; N, 17.48%; O, 20.28%.

Provenance & Evidence