تفاعل #564159

معادلة التفاعل

4-bromomethyl-2,2-difluoro-1,3-benzodioxole

urotropin

water

hydrochloric acid

water

→

2,2-Difluoro-4-formyl-1,3-benzodioxole

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture is heated
2. 2
   درجة الحرارةunder reflux for 3 hours
3. 3
   درجة الحرارةthe mixture is heated for a further 3 hours
4. 4
   أخرىremoved from the receiver
5. 5
   استخلاصAfter extraction with methylene chloride
6. 6
   أخرىthe aldehyde is separated off
7. 7
   workup.DISTILLATIONdistilled

الإجراء التجريبي

117 g of crude 4-bromomethyl-2,2-difluoro-1,3-benzodioxole are added to 120 g of urotropin in 250 ml of water and the mixture is heated under reflux for 3 hours. 120 ml of hydrochloric acid in 150 ml of water are then added and the mixture is heated for a further 3 hours. The crude product is then driven over with steam, removed from the receiver and shaken with 100 g of sodium bisulphate in 250 ml of water. After extraction with methylene chloride, the aqueous phase is acidified with 2N sulphuric acid and the aldehyde is separated off and distilled. The yield is 53 g.

المصدر