1-amino-4-(4-amino-2-sulphoanilino)-9,10-dihydro-9,10-dioxoanthracene-2-sulphonic acid synthesis
- Product Name:1-amino-4-(4-amino-2-sulphoanilino)-9,10-dihydro-9,10-dioxoanthracene-2-sulphonic acid
- CAS Number:18791-01-0
- Molecular formula:C20H15N3O8S2
- Molecular Weight:489.4784
Yield:18791-01-0 43.3%
Reaction Conditions:
Stage #1: sodium 1-amino-4-bromoanthraquinone-2-sulfonatewith sodium carbonate;sodium sulfite in water at 35; for 0.5 h;
Stage #2: 2,5-diaminobenzenesulfonic acidwith copper(l) chloride in water; for 0.5 h;
Stage #3: with copper(l) chloride in water; for 0.5 h;
Steps:
1 Preparation Example 1 Preparation of Compound of [Chemical Formula 2-1]
Preparation Example 1 Preparation of Compound of [Chemical Formula 2-1] After dispersing 10 g of sodium bromaminate (24.7 mmol, 1 eq) in 100 mL of distilled water, 6.3 g of sodium carbonate and 1.3 g of sodium sulfite were added. After stirring at 35° C. for 30 minutes, 5.2 g of 2,5-diaminobenzenesulfonic acid (24.7 mmol, 1 eq) was added. After stirring further for 30 minutes, 0.1 g of copper chloride was added. After stirring further for 30 minutes and filtering, the filtrate was distilled under reduced pressure. A compound represented by [Chemical Formula 2-1] was obtained by purifying the obtained compound by reverse-phase column chromatography (5.23 g, 43.3%). Rf=0.45 (RP-18C, acetonitrile:distilled water=1:3 v/v).
References:
US9512315,2016,B2 Location in patent:Page/Page column 18
