4,4-DIAMINO-2,2'-DICHLORODIPHENYL DISULFIDE synthesis
- Product Name:4,4-DIAMINO-2,2'-DICHLORODIPHENYL DISULFIDE
- CAS Number:729-41-9
- Molecular formula:C12H10Cl2N2S
- Molecular Weight:285.19
Yield:729-41-9 71%
Reaction Conditions:
Stage #1: 3,4-dichloronitrobenzenewith sodium sulfide;sulfur in water at 90; for 5 h;Heating / reflux;
Stage #2: carbon dioxide pH=5.5;
Steps:
Bis(4-amino-2-chlorophenyl)disulfide
76.8 g (0.4 mol) of 1,2-dichloro-4-nitrobenzene, suspended in 120 ml of water, were heated to 90° C. and treated with a solution of 62.4 g (0.8 mol) of sodium sulfide and 12.8 g (0.4 mol) of sulfur in 200 ml of water. After refluxing the mixture for 5 hours, 6 g of carbon dioxide were bubbled through the solution, followed by a regular stream of air. The pH was adjusted to 5.5, the mixture was cooled to room temperature and the resulting precipitate was collected by filtration. The crude material was recrystallized from isopropanol to give 45 g (71%) of the desired product. M+H+=318. LC/MS retention time=1.526.
References:
US2004/248884,2004,A1 Location in patent:Page 99
20201-04-1
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