反应详情

温度

65 °C

A mixture of 3-(6-methoxy-m-tolyl)-5-nitro-1,2-benzisothiazole (63.0 g, 0.210 mol), 5% acetic acid (1.52 L, 1.21 mol) and ethyl acetate (975 mL) is heated to 65° C., treated portionwise with iron powder (58.6 g, 1.05 mol), stirred at 65° C., and filtered through quartz filter paper. The filtrate phases are separated and the aqueous phase is extracted with ethyl acetate. The organic phase and extracts are combined, washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to obtain the title product as an orange oil (55.7 g, 98.1%) which is identified by NMR spectral analyses.

1. filtrationfiltered through quartz
2. filtrationfilter paper
3. customThe filtrate phases are separated
4. extractionthe aqueous phase is extracted with ethyl acetate
5. washwashed sequentially with water and brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo