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CAS No. : | 130-14-3 | MDL No. : | MFCD00064964 |
Formula : | C10H7NaO3S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HIEHAIZHJZLEPQ-UHFFFAOYSA-M |
M.W : | 230.22 | Pubchem ID : | 23661867 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* 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 |
---|---|---|
EXAMPLE 31 1 g of the dye C.I. Disperse Blue 165 prepared as described in Example 1 and 0.2 g of the dye C.I. Disperse Red 184 prepared as described in Example 30 are dispersed in 2,000 g of water. The dispersion is admixed with 4 g of ammonium sulphate, 2 g of a commercial dispersant based on a condensation product of sodium naphthalenesulphonate and formaldehyde and 2 g of a condensation product of m-cresol, formaldehyde and sodium sulphite and adjusted with acetic acid to pH 5.5. | ||
The dispersion is admixed with 4 g of ammonium sulphate, 2 g of commercial dispersant based on a condensation product of sodium naphthalenesulphonate and formaldehyde and 2 g of a condensation product of m-cresol, formaldehyde and sodium sulphite and brought to pH 5.5 with acetic acid. | ||
(d) 2.34 g of the dyestuff obtained in Example 1c are dispersed in 2,000 g of water. The dispersion is admixed with 4 g of ammonium sulphate, 2 g of a commercially available dispersant based on a condensation product of sodium naphthalenesulphonate and formaldehyde and 2 g of a condensation product of m-cresol, formaldehyde and sodium sulphite and is brought to pH 5.5. with acetic acid. |
EXAMPLE 1 14.7 g of the dyestuff of the formula IX STR9 9.5 g of the dyestuff of the formula X STR10 and 5.1 g of the dyestuff of the formula XI STR11 are homogemnsed together with 227.6 g of water, 86.8 g of a higher molecular weight ligninsulphonate and 6.3 g of an arylpolyglycol ether using a dissolver disc, and the pH is brought to 8.0 with 2.6 ml of 50% strength acetic acid. This mixture is then ground down to a fine division of <5 mum in a water-cooling bead mill and the resulting ground paste is sieved to remove the grinding agent and then dried with a spray-drier. 1.25 g of the dyestuff thus obtained are dispersed in 2,000 g of water. 4 g of ammonium sulphate, 2 g of a commercially available dispersing agent based on a condensation product of sodium naphthalenesulphonate and formaldehyde and 2 g of a condensation product of m-cresol, formaldehyde and sodium sulphite are added to the dispersion and the pH is brought to 5.5 with acetic acid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 mi concentrated (95-98%) sulfuric acid. 31.2 G unsubstituted quinacridone (CROMOPHTALS RED 2020, Ciba Specialty Chemicals Inc.) is added at a temperature below 45C and the mixture is stirred for 10 minutes at 40-45C to dissolve the pigment. 39.7 G of a wet naphthalene SULFONIC acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% <strong>[532-02-5]2-naphthalene sulfonic acid sodium salt</strong> (Shanghai Shen Li Chemical Factory) is added at a temperature below 45C and the mixture is stirred for 15 minutes at 40 to 45C followed by the rapid addition of 3.2 G para formaldehyde. The reaction mixture is stirred for one hour at 58-60C, then poured into 2.5 I of ice water. The violet precipitate is stirred for 1 hour at 5-20 C, then filtered. The residue is washed with water to a pH of 2.5 and kept as presscake with a solid content of 13% by weight. Around 0. 5 G of the press cake are reslurried in 20 mi hot water yielding a bluish red colored liquid. It is filtered to remove little aggregated material. The filtrate is red and appears a dye solution. However, the electron micrograph shows the quinacridone in nanosize particle form with an average particle size of 4 to 25 nm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 ml concentrated (95-98%) sulfuric acid. 15 g C. I. Pigment Blue 60 (CIBANONE Blue RS PT 9860, Ciba Specialty Chemicals Inc.) are added at a temperature below 45oC and the mixture is stirred for 15 minutes at 40-45oC to completely dissolve the pigment. 10.7 g of a wet naphthalene sulfonic acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene sulfonic acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature below 50oC and the mixture is stirred for 10 minutes at 40-450C FOLLOWED by the rapid addition of 1.6 g para formaldehyde. The reaction mixture is stirred for one hour at 60-65oC then poured into 2.5 liter ice water. The dark bluish precipitate is stirred for 1 hour at 5-20oC, and then filtered. The dark bluish press cake is washed with water to a pH of 1.5-3. 0 and kept as presscake. About 0.5 g of the press cake are RESLURRIED in 20 ml hot water yielding a blue colored liquid which is filtered through paper to remove little aggregated material. The filtrate is blue and appears like a dye solution. However, the electron micrograph shows the indanthrone pigment in nanosize particle form with an average particle size of from 10 to 30 nm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 250 mi concentrated (95-98%) sulfuric acid. 19.5 g 2, 9-dichloroquinacridone pigment (CINQUASIAO Magenta RT-265-D, Ciba Specialty Chemicals Inc.) are added at a temperature of 50oC and the mixture is stirred for 20 minutes at 48-52oC to dissolve the pigment. 19.9 g of a wet naphthalene sulfonic acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene sulfonic acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature BELOW 50oC and the mixture is stirred for 30 minutes at 45-50oC followed by the rapid addition of 1.6 G PARAFORMALDEHYDE. The reaction mixture is stirred for one hour at 58-60oC then poured into 2.5 liter ice water. The violet precipitate is stirred for 1 hour at 5-20oC, and then filtered. The violet press cake is washed with little water to a pH of 1.5-2. 5 and kept as presscake. About 0.5 g of the press cake are RESLURRIED in 20 ml hot water, yielding a violet colored liquid which is filtered through paper to remove little aggregated material. The filtrate is violet and appears like a dye solution. However, the electron micrograph shows the 2, 9-dichloroquinacridone in nanosize particle form with an average particle size of from 10 to 25 nm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 ml concentrated (95-98%) sulfuric acid. 17 G 2, 9-DIMETHYLQUINACRIDONE pigment (CROMOPHTALS PINK PT, Ciba Specialty Chemicals Inc.) is added at a temperature below 45oC and the mixture is stirred for 10 minutes at 40-45oC to completely dissolve the pigment. 19.9 g of a wet naphthalene sulfonic acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene sulfonic acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature BELOW 45oC and the mixture is stirred for 30 minutes at 40-45oC followed by the rapid addition of 1.6 g para formaldehyde. The reaction mixture is stirred for one hour at 58-60oC then poured into 2.5 liter ice water. The bluish violet precipitate is stirred for 1 hour at 5-20oC, and then filtered. The violet press cake is washed with water to a pH of 2-2.5 and kept as presscake. About 0.5 g of the press cake are reslurried in 20 ML hot water yielding a magenta colored liquid which is filtered through paper to remove little aggregated material. The filtrate is magenta and appears like a dye solution. However, the electron micrograph shows the 2, 9-dimethyl quinacridone in nanosize particle form with an average particle size of from 10 to 30 nm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 150 mi concentrated (95-98%) sulfuric acid. 14 g 2,9-dimethoxyquinacridone are added at a temperature below 45oC and the mixture is stirred for 10 minutes at 40-45oC to completely dissolve the pigment. 15 g of a wet naphthalene sulfonic acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene sulfonic acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature below 45oC and the mixture is stirred for 15 minutes at 40 to 45oC followed by the rapid addition of 1.2 g para formaldehyde. The reaction mixture is stirred for one hour at 58-60oC then poured into 2.5 liter ice water. The bluish violet precipitate is stirred for 1 hour at 5-20oC, then filtered. The bluish violet press cake is washed with water to a pH of 2-2.5 and kept as presscake. About 0.5 g of the press cake are reslurried in 20 ml hot water, yielding a bluish violet colored liquid which is filtered through paper to remove little aggregated material. The filtrate is bluish violet and appears like a dye solution. However, the electron micrograph shows the 2,9-dimethoxyquinacridone in nanosize particle form with an average particle size of from 10 to 30 nm. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 ml concentrated (95-98%) sulfuric acid. 31.2 G unsubstituted quinacridone (CROMOPHTALO Red 2020, Ciba Specialty Chemicals Inc.) are added at a temperature BELOW 45C and the mixture is stirred for 10 minutes at 40-45C to dissolve the pigment. 39.7 G of a wet naphthalene sulfonic acid sodium SALT PRESSCAKE with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene SULFONIC acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature below 45C and the mixture is stirred for 15 minutes at 40-45C followed by the rapid addition of 3.2 G para formaldehyde. The reaction mixture is stirred for one hour at 58-60C then poured into 2. 5 1 ice water. The violet precipitate is stirred for 1 hours at 5-20C, then filtered. The violet press cake is washed with water to a pH of about 2.5 and kept as presscake. About 0.5 G of the press cake are RESLURRIED in 20 mi hot water yielding a red colored liquid which is filtered through paper to remove little aggregated material. The filtrate is red and appears like a dye solution. However, the electron micrograph shows the quinacridone in nanosize particle form with an average particle size of 4 to 25 nm. A small sample of the violet presscake is further washed to a pH of 5 and dried and analytically tested by MALDI. When measured in positive mode, it shows as main component quinacridone (m/z 314 peak), and only a trace of naphthalene SULFONIC acid methyl quinacridone (m/z 535 peak) is found as shown in Figure 1. When measured in negative mode, again the quinacridone is visible (m/z 312 peak) and the polymeric structure of the naphthalene sulfonic acid-formaldehyde polymer is clearly visible with the main molecular weight peaks at 428,649, 870,1091, 1312, 1534,1755 and 1976. The negative mode MALDI spectrum is shown in Figure 2. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A one-liter flask equipped with a stirrer, thermometer, condenser and drying tube is charged with 200 ml concentrated (95-98%) sulfuric acid. 21.4 g C. I. Pigment Red 254 (IRGAZINO DPP Red BO, CIBA Specialty Chemicals Inc.) is added and the mixture is stirred for 1 hour at 55-58oC. 23.9 G of a wet naphthalene sulfonic acid sodium salt presscake with a solid content of 58%, a mixture containing 80% 1-naphthalene sulfonic acid sodium salt and 20% 2- naphthalene sulfonic acid sodium salt (Shanghai Shen Li Chemical Factory) are added at a temperature below 70oC and the mixture is stirred for 10 minutes at 70oC followed by the rapid addition of 1.9 G para formaldehyde. The reaction mixture is stirred for one hour at 70-75oC, then poured into 2.7 liter ice water. The violet brownish precipitate is stirred for 1 hour at 5-20oC, then filtered. The press cake is washed with water to a pH of 2.0-3. 0 and kept as presscake. About 0.5 g of the press cake are reslurried in 20 ml hot water yielding a violet colored liquid which is filtered through paper to remove little aggregated material. The filtrate is brown and appears like a dye solution. However, the electron micrograph shows the diketopyrrolo pyrrole pigment in nanosize particle form with an average particle SIZE OF 10 TO 30 NM. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hexaflorophosphate; In water; | General procedure: D2 (178 mg, 0.5 mmol) was dissolved in water (40 mL) andaddition of aqueous sodium salt of the corresponding anion(0.5 mmol) afforded precipitates which were filtered off, washedwith water and dried. Then the powders were obtained after driedunder vacuum. All salts were dried in a vacuum for 24 h to removesolvents before characterizing them byNMRand elemental analysis |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
3.7 kg | Preparation of Oxoiminium Salt, Hemi-Toluene Solvate: In accordance with Scheme F, L-Valinol (2.6 Kg, 25.2 mol) was melted at 50 C. and (3S,5R,6R)-3-allyl-5-(3-chlorophenyl)-6-(4-chlorophenyl)-3-methyltetrahydro-2H-pyran-2-one (3.6 Kg, 84.0 wt %, 80.8% ee, 7.9 mol) was added. The mixture was heated to 110 C. and agitated at that temperature for 5 h. The mixture was cooled to 20 C. and dichloromethane (17.9 L) was added. Aqueous 1N hydrochloric acid (18.5 L) was added and the biphasic mixture was agitated for 10 min. The phases were separated and the organic phase was washed with an aqueous sodium chloride solution (20 wt %, 7 L). The organic phase was distilled under atmospheric pressure to produce a distillate mass of 13.7 Kg while simultaneously adding dichloromethane (3.3 L). The organic phase was added over the course of 10 min to a solution of p-toluene sulfonic anhydride (5.9 Kg, 18 mol) in dichloromethane (23.0 L). 2,6-Lutidine (3.56 Kg, 33.2 mol) was added over the course of 1 h, maintaining the temperature of the mixture below 25 C. The mixture was agitated at 20 C. for 40 min. The mixture was distilled under atmospheric pressure and at 40 C. to produce a distillate mass of 13.0 Kg. The mixture was added to aqueous 2N sulfuric acid (19.5 Kg) over the course of 15 min, maintaining the temperature below 20 C. The mixture was agitated for 15 min and the phases were separated. The organic phase was washed twice with an aqueous sodium 1-naphthylsulfonate solution (10 wt %, 19.4 Kg), and once with an aqueous sodium bicarbonate solution (5 wt %, 19.5 Kg). 1-naphthylsulfonic acid dihydrate (64 g, 0.26 mol) was added. The organic phase was distilled under reduced pressure and maintaining a temperature of 50 C. to produce a distillate mass of 39.9 Kg while simultaneously adding toluene (27.0 L). The mixture was seeded with oxoiminium salt, hemi-toluene solvate (40 g, 0.06 mol) and agitated for 20 min (The seed material was prepared via the same process in a previously conducted smaller scale experiment). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
0.68 g | In methanol; water; | 4.6 g of sodium 1 -naphthalenesulfonate (manufactured by Tokyo Chemical Industry Co., Ltd.) was dissolved in 100 mE of watet To 100 mE of the obtained aqueous sodium 1 -naphthalenesulfonate solution was added drop- wise a methanol solution formed by dissolving TAMOO5-Cl (0.73 g) in 10 mE of methanol. The precipitated crystals were collected by filtration, these crystals were dissolved in 10 mE of methanol, and the solution was added dropwise to100 mE of the aqueous sodium 1 -naphthalenesulfonate solution. The precipitated crystals were collected by filtration to obtain 0.68 g of TAMO11. It was found to be as follows: MAEDI-MASS (posi): 690.4, and MAEDI-MASS (nega): 207.0. The Xmax (ethyl acetate solution) of the absorption spectrum was 563 nm. |
Tags: 130-14-3 synthesis path| 130-14-3 SDS| 130-14-3 COA| 130-14-3 purity| 130-14-3 application| 130-14-3 NMR| 130-14-3 COA| 130-14-3 structure
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