反应详情

温度

40 °C

145 g of 2,4-dimethoxy-5-chlorosulphonyl benzoic acid, 393 ml of acetic acid and 230.5 g of tin are placed in a 6 liter flask fitted with an agitator, a thermometer and a dropping funnel, and the thick suspension is heated to 40° C. 1,009 ml of hydrochloric acid (density 1.18) is added drop by drop while cooling so as to keep the temperature at from 40° to 45°. The reaction is exothermic. The suspension dissolves gradually, the more acid is added, but the tin salts are precipitated about midway through the adding process. When all the acid has been added the water bath is heated to 55°-60° until the tin has dissolved. 2 liters of water is added and the acid which has precipitated is drained and washed with 460 ml of 10% hydrochloric acid, then with water. It is immediately re-dissolved in water and the necessary soda, the solution is filtered with charcoal, and the acid is re-precipitated by adding concentrated hydrochloric acid. The precipitate is drained, washed with water and dried in an oven at 40°.

1. customfitted with an agitator
2. temperaturewhile cooling so as
3. customat from 40° to 45°
4. dissolutionThe suspension dissolves gradually
5. additionthe more acid is added
6. customthe tin salts are precipitated about midway through the adding process
7. additionWhen all the acid has been added the water bath
8. temperatureis heated to 55°-60° until the tin
9. dissolutionhas dissolved
10. addition2 liters of water is added
11. customthe acid which has precipitated
12. washwashed with 460 ml of 10% hydrochloric acid
13. dissolutionIt is immediately re-dissolved in water
14. filtrationthe necessary soda, the solution is filtered with charcoal
15. customthe acid is re-precipitated
16. additionby adding concentrated hydrochloric acid
17. washwashed with water
18. customdried in an oven at 40°