반응 #7633

반응 방정식

3-bromobenzonitrile

ammonium chloride

trimethylaluminium

methanol

→

3-Bromobenzenecarboximidamide hydrochloride

용매

toluene

hexane

반응 조건

후처리

1. 1
   workup.STIRRINGthe mixture is stirred at 80° C. bath temperature over night
2. 2
   온도It is then cooled down to 0° C.
3. 3
   workup.STIRRINGwith subsequent stirring of 1 hour at room temperature
4. 4
   여과After filtration
5. 5
   세척the solid is washed with methanol for several times
6. 6
   기타the solution is evaporated to dryness in vacuo
7. 7
   세척the residue washed with methanol

실험 절차

1.18 g (22 mmol, 2 equiv.) ammonium chloride are suspended in 40 ml of dry toluene under an argon atmosphere, and the mixture is cooled to 0° C. 11 ml (22 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 2.0 g (11 mmol, 1 equiv.) 3-bromobenzonitrile, the mixture is stirred at 80° C. bath temperature over night. It is then cooled down to 0° C. and 50 ml of methanol are added with subsequent stirring of 1 hour at room temperature. 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.

출처