2,2'-Dithiobis(5-nitrobenzoic acid) synthesis

Yield:1170-38-3 75.5%

Reaction Conditions:

with sodiumsulfide nonahydrate;sulfur in water at 60 - 70; pH=10; for 5 h;

Steps:

2 Synthesis of 2,2'-dithiobis (5-nitrobenzoic acid)

Dissolve 8.0 mmol of Na 2 S · 9H 2 O in 20 mL of water,Add 10mmol sulfur powder, heated to reflux the reaction liquid was reddish brown, hot filtered Na2S2 aqueous solution. Then, the above solution was added dropwise to 15 mL of a basic aqueous solution of pH = 10 dissolved in 10 mmol of 2-chloro-5-nitrobenzoic acid at a controlled temperature of 60 to 70 ° C for 5 hours and then cooled to adjust the pH of the reaction solution About 3, for 2 hours, precipitated dark yellow precipitate, suction filtration, washing, drying yellow powder product. Yield 75.5%

References:

CN103739532,2017,B Location in patent:Paragraph 0025-0027