反应详情

To a solution of 5-chloro-2-nitrobenzyl alcohol (80 g, 0.42 mol) and triethylamine (64 ml, 0.46 mol) in dichloromethane (840 ml) was added drop wise thionyl chloride (34 ml, 0.46 mol) during a period of 30 minutes while the internal temperature was kept below 32° C. by cooling with a water bath. The reaction mixture was stirred for 3 h. The solvent was evaporated and the residue was triturated in warm tert-butyl methyl ether (970 ml). The ammonium salts were removed by filtration and the filtrate was concentrated in vacuo to give the title compound (85 g, 99%) as brown oil which was used in the next step without purification. MS m/e: 205 (M+).

1. customwas kept below 32° C.
2. temperatureby cooling with a water bath
3. customThe solvent was evaporated
4. customthe residue was triturated in warm tert-butyl methyl ether (970 ml)
5. customThe ammonium salts were removed by filtration
6. concentrationthe filtrate was concentrated in vacuo