2-Amino-5-nitrophenol synthesis
- Product Name:2-Amino-5-nitrophenol
- CAS Number:121-88-0
- Molecular formula:C6H6N2O3
- Molecular Weight:154.12
Yield:121-88-0 103.7 kg ，99-57-0 4.1 kg
Reaction Conditions:
Stage #1:2-Benzoxazolinone with sulfuric acid;nitric acid in dichloromethane at 35 - 45;Large scale;
Stage #2: with sodium phosphate dibasic dodecahydrate in water; pH=8 at 100 - 105; under 1125.11 - 1875.19 Torr;Large scale;
Steps:
5.1; 5.2 Example 5. Synthesis of 2-Amino-5-nitrophenol (XIII) and 2-Amino-4-nitrophenol (XIV)
1) Compound (XII)135.1 kg of 99.3% pure 2-benzoxazolone (VI) obtained by the procedure of Example 1 was mixed with 400 kg of dichloromethane, 200 kg of 98% sulfuric acid was added, and stirred, and 355.65% of the mixture was added at 35 to 45 ° C. % nitric acid, the reaction is completed; the layer is allowed to stand to obtain a mixed solution of the compound (XII)-dichloromethane; the dichloromethane is desolvated to obtain 188.3 kg of a distillation residue, wherein the main component is the compound (XII);2) Synthesis of 2-amino-5-nitrophenol (XIII) and 2-amino-4-nitrophenol (XIV)Mixing 188.3 kg of the distillation residue obtained in the first step with 550 kg of water, adjusting the pH of the system to 8 , stirring, heating to 100-105 ° C, and reacting to the end point under the condition of 0.15-0.25 MPa. Cooling to room temperature, solid-liquid separation, obtaining 131.4 kg of a mixture of 2-amino-5-nitrophenol (XIII) and 2-amino-4-nitrophenol (XIV) having a purity of 99.0%, the yield of the mixture is 85.3%;A mixture of the above 2-amino-5-nitrophenol (XIII) and 2-amino-4-nitrophenol (XIV) is crystallized stepwise in an appropriate ratio and an appropriate amount of an ethanol-water system to obtain a purity of 103.7 kg. 99.4% of 2-amino-5-nitrophenol (XIII) and 4.1 kg of 2-amino-4-nitrophenol (XIV) having a purity of 99.8%; the crystallization mother liquor was applied.
References:
Shao Yutian CN110156712, 2019, A Location in patent:Paragraph 0073-0077
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