反応 #94312

反応方程式

8-amino-1,3,6-naphthalenetrisulfonic acid trisodium salt

sodium acetate trihydrate

3-nitrosulfobenzoic anhydride

→

8-(3-nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium salt

溶媒

water

water

反応条件

後処理

1. 1
   workup.STIRRINGThe mixture is stirred at room temperature for 21/2 hours
2. 2
   ろ過filtered
3. 3
   温度The filtrate is cooled
4. 4
   workup.ADDITIONan diluted with ethanol
5. 5
   ろ過The pink solid is collected by filtration
6. 6
   洗浄washed with 85% ethanol, ether
7. 7
   その他dried
8. 8
   濃縮The filtrate is concentrated to a low volume
9. 9
   workup.ADDITIONdiluted with ethanol giving a second crop which
10. 10
    その他is collected

実験手順

To a solution of 20.0 g of 8-amino-1,3,6-naphthalenetrisulfonic acid trisodium salt and 8.75 g of sodium acetate trihydrate in 180 ml of water at room temperature is added 12.0 g of 3-nitrosulfobenzoic anhydride with stirring. A 400 ml portion of water is added. The mixture is stirred at room temperature for 21/2 hours and then filtered. The filtrate is cooled, acidified with 2-3 ml of concentrated hydrochloric acid an diluted with ethanol. The pink solid is collected by filtration, washed with 85% ethanol, ether and dried. The filtrate is concentrated to a low volume and diluted with ethanol giving a second crop which is collected and combined with the first crop giving a total of 27.6 g of 8-(3-nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium salt.

出典