potassium 9,10-dihydro-9,10-dioxoanthracene-1-sulphonate synthesis
- Product Name:potassium 9,10-dihydro-9,10-dioxoanthracene-1-sulphonate
- CAS Number:30845-78-4
- Molecular formula:C14H9KO5S
- Molecular Weight:328.38
Yield:-
Reaction Conditions:
with hydrogenchloride;sodium hydroxide in methanol;water;
Steps:
17 EXAMPLE 17
EXAMPLE 17 150 parts of NaOH are dissolved in 600 parts by volume of methanol at the boil and 333 parts of potassium anthraquinone-1-sulphonate (90% strength) are introduced into this solution with intensive stirring, at 40°-45°C, at such speed that the melt always remains easy to stir (about 30 minutes required). The mixture is now stirred for approximately a further 48 hours at 45°C, until only small amounts of starting material are still present in a sample which is withdrawn and chromatographed. The mixture is diluted with 500 parts of cold water and acidified with 350 parts by volume of concentrated hydrochloric acid whilst cooling with ice, and the product is filtered off, washed with hot water at 90°-100°C until neutral and dried at 100°-120°C. 204 parts of 97% strength 1-methoxy-anthraquinone (90% of theory), still containing 1.3% of 1-hydroxy-anthraquinone, are obtained.
References:
US3971812,1976,A
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