Methanol → 3-Bromobenzene-1-carboximidamide hydrochloride

温度

0 °C

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.

1. stirringthe mixture is stirred at 80° C. bath temperature over night
2. temperatureIt is then cooled down to 0° C.
3. stirringwith subsequent stirring of 1 hour at room temperature
4. filtrationAfter filtration
5. washthe solid is washed with methanol for several times
6. customthe solution is evaporated to dryness in vacuo
7. washthe residue washed with methanol

ORDレコード

ord-adc6fca9416e4444a84e843c2bdf93a5

出典データセット

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07087605B2