反应详情

4.8 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine, 8.4 g of N-iodosuccinimide, 5.2 g of potassium carbonate and 120 ml of methanol were stirred at 23° C. for 20 hours. Most of the methanol was removed by distillation and then a solution of 7 g of Na2S2O3 pentahydrate in 200 ml of water was added, after which the mixture was extracted three times with 100 ml of tert-butyl methyl ether each time. The combined organic phases were washed with 50 ml of water, dried over sodium sulfate and concentrated. Yield: 4.9 g (93%) of a colorless oil;

1. customMost of the methanol was removed by distillation
2. additiona solution of 7 g of Na2S2O3 pentahydrate in 200 ml of water was added
3. extractionafter which the mixture was extracted three times with 100 ml of tert-butyl methyl ether each time
4. washThe combined organic phases were washed with 50 ml of water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated