تفاعل #1057446

معادلة التفاعل

diphenyliodonium bromide

nonafluorobutanesulfonic acid

→

diphenyliodonium nonafluorobutanesulfonate

المردود 79.3%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىthe mixture was reacted at room temperature for 2 hours
2. 2
   أخرىThe thus obtained reaction mixture
3. 3
   ترشيحwas filtered
4. 4
   تركيزconcentrated under reduced pressure
5. 5
   أخرىby purifying 6.4 g of the residue by column chromatography [Wako gel, C-200; eluent of methylene chloride/methanol=9/1 (v/v)]

الإجراء التجريبي

To 100 ml of methanol, 3.61 g (0.01 mole) of diphenyliodonium bromide and 1.62 g (0.007 mole) of silver oxide were suspended, then the mixture was reacted at room temperature for 2 hours. To the reaction solution, 4.2 g (0.014 mole) of nonafluorobutanesulfonic acid was added drop-wise at room temperature, followed by reacting at the same temperature for 2 hours while stirring. The thus obtained reaction mixture was filtered and concentrated under reduced pressure, followed by purifying 6.4 g of the residue by column chromatography [Wako gel, C-200; eluent of methylene chloride/methanol=9/1 (v/v)], to obtain 4.6 g of diphenyliodonium nonafluorobutanesulfonate as a colorless crystal. The thus obtained crystal was named acid generator B1. The measurement results of melting point and NMR of acid generator B1 are shown bellow.

المصدر