4,6-Diaminoresorcinol dihydrochloride synthesis
- Product Name:4,6-Diaminoresorcinol dihydrochloride
- CAS Number:16523-31-2
- Molecular formula:C6H10Cl2N2O2
- Molecular Weight:213.06
412914-87-5
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16523-31-2
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Yield:16523-31-2 69 g
Reaction Conditions:
Stage #1: 2-chloro-4,6-diaminoresorcinolwith ammonium hydroxide;hydrogen in ethanol;water at 60 - 70; under 1500.15 - 2250.23 Torr; for 3 h;Inert atmosphere;
Stage #2: with hydrogenchloride in water;Inert atmosphere;Reagent/catalyst;
Steps:
1.2; 1.3 The method for preparing 4,6-diaminolresorcinol dihydrochloride present embodiment has the following steps:
The 100g (0.426mol) of 2-chloro-4,6-dinitroresorcin, 1g of 5wt% palladium on carbon catalyst, 1500mL of ethanol, and purified water was added 300mL hydrogenation reactor of 5L purged with nitrogen three times and then pass into the hydrogen, the hydrogen pressure was kept at 0.3 ~ 0.4MPa, temperature control in 30 ~ 40 °C, the reaction 2h, HPLC control to the disappearance of starting material. 22g was then added at a concentration of 25wt% (0.157mol) of concentrated aqueous ammonia, the hydrogen pressure was kept at 0.2 ~ 0.3MPa, warmed to 60 ~ 70 °C reaction 3h, HPLC control sample to the intermediate 2-chloro-4,6- amino resorcinol disappear. the material pressure to hydrochloric acid solution, and filtered to give 4,6-diamino dihydrochloride crude, recrystallized 69g of a white solid 4,6-diamino resorcinol dihydrochloride boutique, purity of 99.74%, a yield of 75.9%.
References:
CN105461575,2016,A Location in patent:Paragraph 0017; 0018; 0019
125482-22-6
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16523-31-2
149 suppliers
$11.00/250mg
51652-35-8
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16523-31-2
149 suppliers
$11.00/250mg