反应详情

A mixture of 26.0 g of sodium 2-chloro-5-nitrobenzenesulfonate and 5.0 g of sodium silicate (Na2O.nSiO2 ; n=about 3) was suspended in 120 ml of 2-propoxyethanol and while stirring the suspension, a solution prepared by dissolving 5.0 g of sodium hydroxide in 5 ml of water was dropwise added thereto at 65° C. over a period of 10 minutes. After the dropwise addition was completed, the resulting mixture was stirred at 65° C. for 3 hours and insoluble products were then removed by suction filtration. On allowing the filtrate to stand, solids precipitated. The solids were removed by filtration and the filtrate was condensed and dried. The addition of 100 ml of ethanol to the residue resulted in the formation of crystals. The crystals were collected by filtration, washed with isopropyl alcohol and dried at 50° C. Yield: 14.1 g.

1. customa solution prepared
2. additionwas dropwise added
3. additionAfter the dropwise addition
4. stirringthe resulting mixture was stirred at 65° C. for 3 hours
5. custominsoluble products were then removed by suction filtration
6. customsolids precipitated
7. customThe solids were removed by filtration
8. customcondensed
9. customdried
10. additionThe addition of 100 ml of ethanol to the residue
11. customresulted in the formation of crystals
12. filtrationThe crystals were collected by filtration
13. washwashed with isopropyl alcohol
14. customdried at 50° C