반응 #7634

반응 방정식

1-cyanonaphthalene

ammonium chloride

trimethylaluminium

→

1-Naphthalenecarboximidamide hydrochloride

용매

methylene chloride

hexane

toluene

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred at 80° C. bath temperature over night
2. 2
   온도The mixture is cooled
3. 3
   여과After filtration
4. 4
   세척the solid is washed with methanol for several times
5. 5
   기타the solution is evaporated to dryness in vacuo
6. 6
   세척the residue washed with methanol
7. 7
   workup.STIRRINGstirred in a mixture of methylene chloride containing 10% methanol

실험 절차

14 g (261 mmol, 2 equiv.) ammonium chloride are suspended in 150 ml of dry toluene under an argon athmosphere, and the mixture is cooled to 0° C. 130 ml (260 mmol, 2 equiv.) of a 2M solution of trimethylaluminium in hexane are added dropwise, and the reaction mixture is stirred at room temperature until no more evolution of gas is observed. After addition of 20 g (130 mmol, 1 equiv.) 1-cyanonaphthalene, the mixture is stirred at 80° C. bath temperature over night. The mixture is cooled and poured into a slurry of silica in methylene chloride. After filtration, the solid is washed with methanol for several times, the solution is evaporated to dryness in vacuo and the residue washed with methanol. The combined filtrates are pooled and stirred in a mixture of methylene chloride containing 10% methanol.

출처