反应详情

26.0 g of sodium 2-chloro-5-nitrobenzenesulfonate and 5.0 g of sodium silicate (Na2O.nSiO2 wherein n is about 3) were suspended in 120 ml of 2-propoxyethanol. To the suspension was added dropwise with stirring a solution containing 5.0 g of sodium hydroxide dissolved in 5 ml of water at 65° C. for 10 minutes. After completion of the addition, the reaction mixture was stirred at 65° C. for 3 hours and the insoluble materials were removed by filtration under suction. The solids which deposited from the filtrate upon standing were removed by filtration. The filtrate was concentrated to a dry solid. 100 ml of ethanol was added to the residue to form crystals. The crystals were recovered by filtration, washed with isopropyl alcohol and dried at 50° C. Yield: 14.1 g. The compound at first melted at 70° to 74° C., then solidified at about 130° C. and again melted at 206° to 209° C.

1. additionTo the suspension was added dropwise
2. additionAfter completion of the addition
3. stirringthe reaction mixture was stirred at 65° C. for 3 hours
4. customthe insoluble materials were removed by filtration under suction
5. customupon standing were removed by filtration
6. concentrationThe filtrate was concentrated to a dry solid
7. addition100 ml of ethanol was added to the residue
8. customto form crystals
9. filtrationThe crystals were recovered by filtration
10. washwashed with isopropyl alcohol
11. customdried at 50° C
12. customsolidified at about 130° C.