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CAS No. : | 135-53-5 | MDL No. : | MFCD00004074 |
Formula : | C10H7NaO5S | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | JFXDYPLHFRYDJD-UHFFFAOYSA-M |
M.W : | 262.21 | Pubchem ID : | 4410831 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P264-P280-P305+P351+P338+P337+P313 | UN#: | |
Hazard Statements: | H319 | Packing Group: | |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
31% | With Dowex H+ resin; for 42.0h;Heating / reflux; | To a solution of the sulfonate (500 mg, 1.91 mmol) in anhydrous 1-pentanol (50 mL) was added Dowex H+ resin (500 mg). The mixture was refluxed for 42 hrs before filtering. Concentration of the solvent furnished a black gum. The gum was chromatographed on silica (hexanes/EtAc, 2: 1) to furnish the title compound as a light brown solid (183 mg, [31%).] 'H NMR [(CDC13)] : [6] 7.6-7. 11 (bm, [5H,] ArH), 4.2 (t, [2H,-OCH2CH2CH2CH2CH3),] 1.9 (m, [2H,-OCH2CH2CH2CH2CH3),] 1.4 (m, [4H,-OCH2CH2CH2CH2CH3),] 0.9 (t, 3H, [-OCH2CH2CH2CH2CH3)] ; LRMS (ESI): [WALZ] 311 [M+H+] ; [CLSHLSOSS] : 310.37 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With bromine; In acetic acid; | (I) 1,4-Dibromo-2,3-diacetoxy-6-naphthalene sulphonyl chloride To a suspension of 2,3-dihydroxy-6-naphthalene sulphonic acid sodium salt (5.24 g) in acetic acid (100 ml) was added, dropwise over 30 minutes, bromine (2.3 ml) in acetic acid (50 ml). The solution was stirred at room temperature for 16 hours, partially concentrated and ether was added to precipitate 1,4-dibromo-2,3-dihydroxy-6-naphthalene sulphonic acid (8.7 g); delta(DMSO-d6 /TFA-d); 7.72(br d, 1H); 7.99(d,1H); 8.37(br s, 1H). This was acetylated in conventional manner and treated with phosphorus pentachloride as in F (above) to give the title compound; delta(CDCl3); 2.44(s,6H); 8.16(dd,1H); 8.56(d,1H); 9.02(d,1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With acetic acid; In water; | (J) 1,4-Dichloro-2,3-diacetoxy-6-naphthalene sulphonylchloride Chlorine was passed through a solution of 2,3-dihydroxy-6-naphthalene sulphonic acid sodium salt (2.0 g) in water (20 ml) until all starting material had been consumed. Solvent was evaporated and the residue purified by chromatography on Diaion HP 20 SS resin (aqueous methanol with 1% acetic acid) to give 1,4-dichloro-2,3-dihydroxy-6-naphthalene sulphonic acid. This was acetylated in conventional manner and treated with phosphoris pentachloride as in F to give the title compound as a crystalline solid; delta(CDCl3); 2.44 (s,6H); 8.16(dd,1H); 8.55(d,1H); 9.00(d,1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium chloride; sulfuric acid; acetic anhydride; In water; | EXAMPLE 3 Preparation of 2,3-diacetoxy-7-naphthalenesulfonic acid sodium salt A mixture of 72.3 g. (0.276 mole) of <strong>[135-53-5]2,3-dihydroxy-7-naphthalenesulfonic acid sodium salt</strong>, 360 ml. of acetic anhydride and 5 drops of concentrated sulfuric acid was stirred 8 hr. on a steam bath and cooled overnight to room temperature. The solid was collected, washed with acetic anhydride, pressed as dry as possible, dissolved in 400 ml. of water, mixed with 500 ml. of 20% sodium chloride solution and allowed to stand overnight. The solid was collected, washed with 20% sodium chloride and dried to give 69.9 g. (73.1%) of colorless crystals, m.p. 270-300 C. (dec.). Anal. calc'd. for C14 H11 NaO7 S: C, 48.6; H, 3.18; Na, 6.65; S, 9.25. Found: C, 45.7; H, 3.3; Na, 6.4; S, 8.7. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With dimethyl sulfate; In sodium hydroxide; water; | (A) Sodium 6,7-dimethoxy-2-naphthalenesulfonate To a well stirred solution of 70.8 g of <strong>[135-53-5]sodium 6,7-dihydroxy-2-naphthalenesulfonate</strong> and 77.2 g of sodium hydroxide in 450 ml of water was added dropwise 230 ml of dimethyl sulfate at 60 C over a period of one hour, during which the product precipitated. To this reaction mixture was added in portions 38.8 g of sodium hydroxide, and stirring was continued for 1 hour. After one hour at room temperature, the precipitate was filtered, washed with ethanol and dried to give 50 g of sodium 6,7-dimethoxy-2-naphthalenesulfonate. | |
With dimethyl sulfate; In sodium hydroxide; water; | (A) Sodium 6,7-dimethoxy-2-naphthalenesulfonate To a well stirred solution of 70.8 g of <strong>[135-53-5]sodium 6,7-dihydroxy-2-naphthalenesulfonate</strong> and 77.2 g of sodium hydroxide in 450 ml of water was added dropwise 230 ml of dimethyl sulfate at 60 C over a period of one hour, during which time the product precipitated. To this reaction mixture was added in portions 38.8 g of sodium hydroxide, and stirring was continued for one hour. After one hour at room temperature, the precipitate was filtered, washed with ethanol and dried to give 50 g of sodium 6,7-dimethoxy-2-naphthalenesulfonate. | |
With dimethyl sulfate; In sodium hydroxide; water; | (A) Sodium 6,7-dimethoxy-2-naphthalenesulfonate: To a well stirred solution of 70.8 g of <strong>[135-53-5]sodium 6,7-dihydroxy-2-naphthalenesulfonate</strong> and 77.2 g of sodium hydroxide in 450 ml of water was added dropwise 230 ml of dimethyl sulfate at 60 C over a period of one hour, during which time the product precipitated. To this reaction mixture was added in portions 38.8 g of sodium hydroxide, and stirring was continued for 1 hour. After 1 hour at room temperature, the precipitate was filtered, washed with ethanol and dried to give 50 g of sodium 6,7-dimethoxy-2-naphthalenesulfonate. |
With dimethyl sulfate; In sodium hydroxide; water; | (A) Sodium 6,7-dimethoxy-2-naphthalenesulfonate To a well stirred solution of 70.8 g of <strong>[135-53-5]sodium 6,7-dihydroxy-2-naphthalenesulfonate</strong> and 77.2 g of sodium hydroxide in 450 ml of water was added dropwise 230 ml of dimethyl sulfate at 60 C over a period of 1 hour, during which time the product precipitated. To this reaction mixture was added in portions 38.8 g of sodium hydroxide, and stirring was continued for one hour. After one hour at room temperature, the precipitate was filtered, washed with ethanol and dried to give 50 g of sodium 6,7-dimethoxy-2-naphthalenesulfonate. | |
With dimethyl sulfate; In sodium hydroxide; water; | A. Sodium 6,7-dimethoxy-2-naphthalenesulfonate To a well stirred solution of 70.8 g of <strong>[135-53-5]sodium 6,7-dihydroxy-2-naphthalenesulfonate</strong> and 77.2 g of sodium hydroxide in 450 ml of water was added dropwise 230 ml of dimethyl sulfate at 60 C over a period of 1 hour, during which time the product precipitated. To this reaction mixture was added in portions 38.8 g of sodium hydroxide, and stirring was continued for 1 hour. After one hour at room temperature, the precipitate was filtered, washed with ethanol and dried to give 50 g of sodium 6,7-dimethoxy-2-naphthalenesulfonate. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With concentrated hydrochloric acid; sulfuric acid; acetic anhydride; acetic acid; In methanol; thionyl chloride; diethyl ether; dichloromethane; | (a) 6,7-Dihydroxy-naphthalene-2-sulfonic Acid Dipropylamide The suspension of <strong>[135-53-5]2,3-dihydroxynaphthalene-6-sulphonic acid sodium salt</strong> (2.6 g), acetic acid (20 ml), acetic anhydride (10 ml) and sulphuric acid (0.6 ml) was refluxed for 30 minutes. Volatiles were removed under reduced pressure and the remaining solids were refluxed in thionyl chloride (20 ml) for 30 minutes. Volatiles were again evaporated and then methylene chloride (30 ml) and dipropylamine (6.8 ml) added and this mixture stirred at room temperature for two hours. The reaction mixture was washed with 1 M hydrochloric acid (70 ml) and the organic phase evaporated. To the remaining solids were added methanol (100 ml) and concentrated hydrochloric acid (20 ml) and this mixture was stirred at room temperature for 22 hours. Diethyl ether (400 ml) was added and the organic phase was washed three times with water. Ether was evaporated. Yield: 1.3 g. 1H-NMR (DMSO-d6, 400 MHz): 0.81 (t, 6H, J=7 Hz), 1.40-1.52 (m, 4H), 3.03 (t, 4H, J=8 Hz), 7.21 (s, 1H), 7.33 (s, 1H), 7.45 (dd, 1H, J=9 Hz, 2 Hz), 7.75 (d,1H, J=9 Hz), 8.09 (d, 1H, J=2 Hz),), 9.9 (s, 1H), 10.1 (s, 1H). |
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