反应详情

温度

60 °C

250 g of disodium 4-chloro-3-hydroxysulfinylbenzoate were suspended in 500 ml of abs. dimethylformamide at RT, 218 ml of methyl iodide (3.5 mol) were added and the reaction mixture was heated to 60° C. It was subsequently stirred at this temperature for 4 hours, then allowed to stand at RT overnight. The mixture became solid on cooling. It was warmed to 70° C., diluted with 250 ml of abs. dimethylformamide and subsequently stirred at 70° C. for a further 3 hours. The solvent was distilled off, the residue was taken up in 1000 ml of water, stirred for 30 minutes in an ice bath, filtered off with suction and washed 3 times with about 200 ml of water each time, sucked dry and dried in vacuo (50° C.).

1. waitto stand at RT overnight
2. temperatureon cooling
3. temperatureIt was warmed to 70° C.
4. additiondiluted with 250 ml of abs
5. distillationThe solvent was distilled off
6. stirringstirred for 30 minutes in an ice bath
7. filtrationfiltered off with suction
8. washwashed 3 times with about 200 ml of water each time
9. customsucked dry
10. customdried in vacuo (50° C.)