反応 #1663556

反応方程式

1,8-diaminonaphthalene

salicylaldehyde

→

2-(o-hydroxyphenyl)perimidine

溶媒

ethanol

反応条件

後処理

1. 1
   温度heated
2. 2
   温度under reflux for 45 min.
3. 3
   ろ過The mixture is then filtered
4. 4
   洗浄the filtrate is washed with ethanol and ether
5. 5
   workup.ADDITIONThe green solid is treated with heated dimethylformamide (charcoal)
6. 6
   ろ過filtered hot
7. 7
   その他The catalyst is removed from the product by filtration along with the charcoal
8. 8
   温度The yellow-orange filtrate is cooled
9. 9
   workup.ADDITIONupon addition of water

実験手順

To 1,8-diaminonaphthalene (31.6 g, 0.2 mole) suspended in 200 ml absolute ethanol is added salicylaldehyde (24.4 g, 0.2 mole) and 7 g 10% palladium-on-carbon. The mixture is stirred and heated under reflux for 45 min., after which it is allowed to stand for 18 hours at ambient temperature. The mixture is then filtered and the filtrate is washed with ethanol and ether. The green solid is treated with heated dimethylformamide (charcoal) and filtered hot. The catalyst is removed from the product by filtration along with the charcoal. The yellow-orange filtrate is cooled, and upon addition of water, yields the desired product, 2-(o-hydroxyphenyl)perimidine, orange crystals, m.p. 258°-260° dec.

出典