Olive-shaped N-methyl-4-nitrophthalimide crystal and preparation method thereof
A technology of nitrophthalimide and methylphthalimide, applied in the field of N-methyl-4-nitrophthalimide crystal and its preparation, can solve the problem of Nitrification reaction safe feeding, difficulty, low yield and other problems, to avoid heat accumulation, increase yield, improve product yield effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0026] Add 161g of N-methylphthalimide solid into 300g of 98wt% concentrated sulfuric acid with stirring started, and heat the system to 40°C until N-methylphthalimide is completely dissolved. Weigh 65g of 98wt% fuming nitric acid, gradually add fuming nitric acid into the system through the dropping funnel, cool the system with cooling water to remove heat, and keep the system temperature at 40°C. After the nitric acid was added dropwise, keep at 40°C and react for 2.5 hours.
[0027] The reaction system was lowered to normal temperature, poured into 618g of ice-water mixture with stirring, and precipitated. After the product N-methyl-4-nitrophthalimide solid was filtered and washed with water until pH = 7, the product was dried at 90° C. under normal pressure.
[0028] Add the dried product to the washing and purifying solvent, the solvent composition is tributyl phosphate: pyridine: ethyl acetate = 4: 4: 92, N-methyl-4-nitrophthalimide in the system The content accounts f...
Embodiment 2
[0030] Add 161g of N-methylphthalimide solid into 326g of 93wt% concentrated sulfuric acid with stirring started, and heat the system to 40°C until N-methylphthalimide is completely dissolved. Weigh 71.44g of 97wt% fuming nitric acid, gradually add fuming nitric acid into the system through the dropping funnel, cool the system with cooling water to remove heat, and keep the system temperature at 45°C. After the nitric acid was added dropwise, the reaction temperature was kept at 60° C. for 2 hours.
[0031] The reaction system was lowered to normal temperature, poured into 515 g of ice-water mixture with stirring, and precipitated. After the product N-methyl-4-nitrophthalimide solid was filtered and washed with water until pH=7, the product was dried under normal pressure at 100°C.
[0032] The dried product is added to the washing and purifying solvent, and its solvent composition is tripolyphosphate: thiophene: methyl acetate = 1: 3: 96, N-methyl-4-nitrophthalimide in the s...
Embodiment 3
[0034] Add 161g of N-methylphthalimide solid into 306g of 96wt% concentrated sulfuric acid with stirring started, and heat the system to 30°C until N-methylphthalimide is completely dissolved. Weigh 66.3g of 95wt% fuming nitric acid, gradually add fuming nitric acid into the system through the dropping funnel, cool the system with cooling water to remove heat, and keep the system temperature at 30°C. After the nitric acid was added dropwise, the temperature was kept at 30° C., and the reaction was carried out for 3 hours.
[0035] The reaction system was lowered to normal temperature, poured into 824 g of ice-water mixture with stirring, and precipitated. After the product N-methyl-4-nitrophthalimide solid was filtered and washed with water until pH = 7, the product was dried at 80° C. under normal pressure.
[0036] Add the dried product to the washing and purifying solvent, the solvent composition is triphenyl phosphite: indole: ethyl lactate=5:5:90, N-methyl-4-nitrophthalo...
PUM
| Property | Measurement | Unit |
|---|---|---|
| Bulk density | aaaaa | aaaaa |
| Bulk density | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More