Methyl Orange synthesis
- Product Name:Methyl Orange
- CAS Number:547-58-0
- Molecular formula:C14H14N3NaO3S
- Molecular Weight:327.33
121-69-7
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$10.00/25mL
121-57-3
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$13.00/25g
547-58-0
423 suppliers
$14.49/5g
Yield:547-58-0 95.01%
Reaction Conditions:
Stage #1: N,N-dimethyl-anilinewith hydrogenchloride in water;N,N-dimethyl-formamide at 25;
Stage #2: with sodium nitrite in water;N,N-dimethyl-formamide;
Stage #3: 4-aminobenzene sulfonic acid in water;N,N-dimethyl-formamide at 25; for 0.00333333 h;
Steps:
8 Example 8
(1) Take 1.36 g of N,N-dimethylaniline in a 100 mL beaker at room temperature (25°C) and add 15 mL of DMF (N,N-dimethylformamide).2.5mL concentrated hydrochloric acid (37%), 32.5mL deionized water, stirring evenly to obtain the feed liquid A;(2) Take 0.731g of sodium nitrite solid in a 100mL beaker, add 15mL DMF (N, N-dimethylformamide), 35mL of deionized water, and stir until the solid sodium nitrite completely dissolved to prepare the feed solution B;(3) Take the coupling component 1.73g sulfanilic acid in a beaker at room temperature (25°C), add 60mL water,After 30mLDMF (N, N- dimethylformamide) after shaking, adding sodium hydroxide solution to adjust the pH of the coupling component is 10, stirring until the coupling component is completely dissolved to prepare feed solution C; (4) This embodiment used micro-reactor for patents ZL200710177813.8 introduced by the micro-contact mixer, at room temperature (25 °C), in order to feed liquid A as disperse phase, liquid continuous phase B, through containing 16 parallel channel of the double multiple thin layer micro contact mixer the diazotization reaction occurs, for constant flow pump control reaction liquid flow are 35 ml/min, the reaction time is 5 s, obtained D diazonium salt solution; (5) In order to feed liquid C as continuous phase, as disperse phase D diazonium salt solution, at room temperature (25 °C) by containing 20 parallel channel of the double multiple thin layer micro contact mixer generating coupling reaction, for constant flow pump control the feed liquid D C and solution flow rate is 70 ml/min, reaction time is 7 s, at the end of the azo dye aqueous solution. By UV-visible spectrophotometry the dye of the blood standard working curve, then according to the products under the maximum absorption wavelength of absorbance to calculate the concentration of the products, the calculated azo dye product 32 (methyl orange) (structural formula shown in table 1), the yield rate thereof is 95.01%.
References:
CN107488361,2017,A Location in patent:Paragraph 0064-0070
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