N N-DIMETHYL-1 4-PHENYLENEDIAMINE SULFA& synthesis
- Product Name:N N-DIMETHYL-1 4-PHENYLENEDIAMINE SULFA&
- CAS Number:536-47-0
- Molecular formula:C8H14N2O4S
- Molecular Weight:234.27
536-47-0
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![Thiosulfuric acid (H2S2O3), S-[2-amino-5-(dimethylamino) phenyl] ester](/CAS/20211123/GIF/43035-11-6.gif)
43035-11-6
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Yield:43035-11-6 49%
Reaction Conditions:
with potassium dichromate;aluminum(III) sulphate octadecahydrate;sodium thiosulfate;zinc(II) chloride in water at 0 - 10; for 2.5 h;
Steps:
1.a
Example 1 - Preparation of arylthiosulphonic acids: 2-Amino-5- dialkylaminophenylthiosulphonic acid; Λ/,Λ/-Dialkyl-p-phenylenediamine sulphate (130 mmol) was added to a mechanically stirred solution of aluminium sulfate octadecahydrate/water (43.6 g, 65 mmol/100 ml). To this was added sodium thiosulfate/water (22.0 g, 139 mιmol/80 ml) followed by zinc chloride/water (8.8 g, 63 mmol/12 ml). The solution was cooled to 0 0C and potassium dichromate/water (5.0 g, 17 mmol/20 ml) was added dropwise over a 30 minute period. Following this addition, the mixture was allowed to stir for 2 hours. During the last 30 minutes the temperature was allowed to rise to 10 0C causing the formation of a viscous precipitate. This was isolated by filtration and washed with water followed by acetone.; Example 1a; 2-Amino-5-dimethylaminophenylthiosulphonic acid was prepared as above from Λ/,Λ/-dimethyl- p-phenylenediamine sulphate, yield=15.87 g (49%), m.p. 190 0C (dec.)
References:
WO2010/97626,2010,A2 Location in patent:Page/Page column 17-18
536-47-0
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65517-31-9
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536-47-0
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100-04-9
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