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CAS No. : | 135-76-2 | MDL No. : | MFCD00070488 |
Formula : | C10H7NaO4S | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | ZPWQALCOMQRMRK-UHFFFAOYSA-M |
M.W : | 246.22 | Pubchem ID : | 23667648 |
Synonyms : |
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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 |
---|---|---|
Step 1 (VII-1): STR29 124 g (0.5 mol) of <strong>[50594-82-6]3,4,5-trichlorobenzotrifluoride</strong> are added to a stirred mixture of 135 g (0.5 mol) of the sodium salt of 6-hydroxy-naphthalene-2-sulphonic acid, 30 g (0.54 mol) of potassium hydroxide powder and 1,000 ml of dimethyl sulphoxide, and the reaction mixture is stirred first for 3 hours at 60 C. and then for 15 hours at 20 C. After the mixture has been concentrated, the residue is digested with water, and the product which has been obtained in crystalline form is isolated by filtration with suction. This gives 209.5 g (91% of theory) of the sodium salt of 6-(2,6-dichloro-4-trifluoromethyl-phenoxy)-naphthalene-2-sulphonic acid, which melts above 310 C. with decomposition. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A diazo slurry is prepared by dissolving 13.4 parts of 2- AMINONAPHTAHLENE-1-SULFONIC acid in 140 parts of water and 4. 8 parts of 50% sodium hydroxide solution. The solution is cooled to 0 C. by the addition of ice and diazotized by the addition of 17 parts of a 25% solution of sodium nitrite and 22 parts of 20 Baume hydrochloric acid and stirring the slurry at 5- 10 C. for 40 minutes. Excess nitrite is quenched with sulfamic acid. A small amount of an antifoam agent is used to control the foam. A coupler slurry is prepared by dissolving 15.4 parts of sodium salt of 2-hydroxy-naphthalene-6-sulfonic acid (Schaeffer's Salt) in 500 parts of water containing 4.5 parts of 50% sodium hydroxide. Alkylamine-guanidine polyoxyethanol (1.7 parts) is added and the slurry is cooled to 20 C. with ice. The diazo slurry is coupled into the coupler slurry over a period of 30 minutes while maintaining the pH at 6-8. The pH of the slurry is then raised to 9.8 by addition of 10 percent solution of sodium hydroxide and the mixture is stirred 20 minutes. Alkylamine-guanidine polyoxyethanol (1.0 part) is added, the pH is adjusted to 6.5 and 24 parts strontium nitrate are added. The slurry is stirred for 50 minutes at pH 7.5, and heated at a rate of approximately 1 C. /MINUTE TO BOILING AND BOILED FOR TWO HOURS. THE SLURRY IS THEN ICED TO LOWER than 50 C. and filtered ; the filter cake is washed with water, dried overnight at 80 C. and pulverized to give a red pigment powder. Referring to Figure 1, an X-ray diffraction pattern of the Example 1 pigment shows high diffraction intensity at diffraction angles (CT: 2. 0S, SS: 0.020 dg, WL: 1.5406) of 10. 4, 17. 5, 18. 7, 21. 6 and 23, moderate diffraction intensities at 14. 4, 15, 24. 4, 24. 8, 25. 2 and 26. 2 and relatively low diffraction intensities at 15. 4, 17. 5, 17. 8, 19. 3, 20, 21, 21. 8, 26. 6, 28. 6, 30. 2, 31. 6, 32. 1, 34. 8 and 38. The X-ray diffraction pattern indicates that the material is of a crystalline nature. The sharp and accountable peaks of Figure 1 indicate that the pigment of Example 1 made in accordance with the present invention is essentially pure. Example 4 The procedure of Example 1 is repeated except that after alkylamine- guanidine POLYOXYETHANOL is added (second instance) the pH is adjusted to 6 instead of 7.5 to give a red pigment powder. | ||
The procedure of Example 1 is repeated except that 1.7g of bis (2- HYDROXYETHLY) cocamine oxide is added instead of 1.0 part of alkylamine- guanidine polyoxyethanol to give a red pigment powder. Example 3 The procedure of Example 2 is repeated except that after bis (2- HYDROXYETHLY) cocamine oxide is added, the pH is adjusted to 9.2 instead of 7.5 to give a red pigment powder. | ||
Comparative Example 1 The procedure of Example 1 is repeated except that after coupling alkylamine-guanidine polyoxyethanol is not added to give a red pigment powder. Comparative Example 2 The procedure of Example 4 is repeated except that after coupling alkylamine-guanidine polyoxyethanol is not added to give a red pigment powder. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
A diazo slurry is prepared by dissolving 13.4 parts of 2- AMINONAPHTAHLENE-1-SULFONIC acid in 140 parts of water and 4.8 parts of 50% sodium hydroxide solution. The solution is cooled to 0 C. by the addition of ice and diazotized by the addition of 17 parts of a 25% solution of sodium nitrite and 22 parts of 20 Baume hydrochloric acid and stirring the slurry at 5- 10 C. for 40 minutes. Excess nitrite is quenched with sulfamic acid. A small amount of an antifoam agent is used to control the foam. A coupler slurry is prepared by dissolving 15.4 parts of sodium salt of 2-hydroxy-naphthalene-6-sulfonic acid (Schaeffer's Salt) by heating in 500 parts of water containing 4.5 parts of 50% sodium hydroxide. The slurry is cooled to 20 C. with ice. The diazo slurry is coupled into the coupler slurry over a period of 30 minutes while maintaining the pH at 6-8. The pH of the slurry is then raised to 9.8 by addition of 10 percent solution of sodium hydroxide followed by the addition of and 2.5 parts of bis (2-hydroxyethyl) cocamine oxide. The mixture is stirred 20 minutes, pH is adjusted to 8 and 22 parts calcium chloride are added. The slurry is stirred for 50 minutes and heated to boiling at a rate of APPROXIMATELY 1 C. /MINUTE AND BOILED FOR TWO HOURS. THE SLURRY IS THEN ICED to lower than 50 C. and filtered; the filter cake is washed with water, dried overnight at 80 C. and pulverized to give a red pigment powder. Example 2 The procedure of Example 1 is repeated except that after addition of bis (2-hydroxyethyl) cocamine oxide, the pH is adjusted to 6.5 instead of 8 to give a red pigment powder. Example 3 The procedure of Example 1 is repeated except that after addition of bis (2-hydroxyethyl) cocamine oxide, the pH is adjusted to 5 instead of 8 to give a red pigment powder. | ||
The procedure of Example 1 is repeated except that 2 parts of alkylamine-guanidine polyoxyethanol are added instead of 1.7 parts of bis (2- hydroxyethyl) cocamine oxide to give a red pigment powder. Example 5 The procedure of Example 4 is repeated except that after addition of alkylamine-guanidine polyoxyethanol, the pH is adjusted to 6.5 instead of 8 to give a red pigment powder | ||
The procedure of Example 1 is repeated except that bis (2- hydroxyethyl) cocamine oxide is not added to the reaction mixture to give a red pigment powder. Comparative Example 2 The procedure of Comparative Example 1 is repeated except that before the addition of calcium chloride, the pH is adjusted to 6.5 instead of 8 to give a red pigment powder. |
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