反应详情

温度

25 °C

59 g of sodium 2-(2-methoxyethoxy)-5-nitrobenzenesulfonate prepared as described in Example 1 above was added to a mixture of 200 ml of acetone and 75 ml of phosphorus oxychloride. 75 ml of N,N-dimethylacetamide was added dropwise to the mixture with stirring while the reaction mixture was maintained at 30° to 40° C. After the completion of the addition, the mixture was allowed to stand with stirring until it cooled to room temperature (25° C.). The reaction mixture was then poured into 600 ml of ice water (0° C.), stirred for 30 minutes and the crystals thus-precipitated were recovered by filtration. The crystals were washed with water and air-dried. Yield: 56 g; Melting Point: 74° to 74.5° C.

1. temperaturewas maintained at 30° to 40° C
2. additionAfter the completion of the addition
3. stirringwith stirring until it
4. stirringstirred for 30 minutes
5. customthe crystals thus-precipitated
6. filtrationwere recovered by filtration
7. washThe crystals were washed with water
8. customair-dried