反应详情

温度

50 °C

153 g of tin dichloro dihydrate (678 mmol) are added to 1.7 l of conc. HCl and heated to about 50° C. 26 g (113 mmol) of 2-bromo-1,3-dimethyl-5-nitrobenzene (Example II) are added. The suspension is heated at about 70° C. for 20 min. It is then allowed to cool slowly to room temperature. The precipitated white solid is filtered off and washed with cold acetone. The resulting hydrochloride is taken up in 1 N NaOH, briefly stirred and extracted 5 times with ethyl acetate. The organic phases are combined and dried over sodium sulphate, and the solvent is removed in vacuo.

1. temperatureThe suspension is heated at about 70° C. for 20 min
2. temperatureto cool slowly to room temperature
3. filtrationThe precipitated white solid is filtered off
4. washwashed with cold acetone
5. extractionextracted 5 times with ethyl acetate
6. dry with materialdried over sodium sulphate
7. customthe solvent is removed in vacuo