Extracts from JACS, 51, (1969), 143-144
Procedure #1:
In a 5-l., 4-necked round-bottom flask fitted with a stirrer, condenser and a thermometer, 428.7 g of Mn(OAc)2 . 4H2O in 3 l of GAA was heated to 110°C. Ground KMnO4 (68.2 g) was added in small portions through the condenser over a 20 min. period, while the temperature was mantained at 110°C. The rxn mixture was heated an additional 20 min., cooled, poured into water (750 mL), and left to crystallize overnight. The solid was filtered off, washed with ether and air dried. Yield: 486 g (82%)
Procedure #2: (FOR THE ANHYDROUS PRODUCT)
A mixture of Mn(NO3)2 . 6H2O (60 g) and Ac2O (225 mL) was stirred vigorously in a 4-l. beaker and heated cautiously until the cloudy mixture suddenly turned clear. The heating was stopped and a vigorous rxn followed during which there was a copious evolution of NO2. The product was allowed to crystallize overnight, filtered, washed with Ac2O, and dried over P2O5. The Mn(OAc)3 anhydrous thus obtained titrated as 90-98% Mn(OAc)3. Yield: 70-90%.