Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Urea | HCID 1176 | — |
| Reactant | 2-Methylimidazole | HCID 12749 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178433402 | HCID 178433402 | 81.5% |
Reaction Steps
A mixture of 2,730 parts of sulfuric acid (35 percent by weight), 835 parts of 2-methylimidazole, 410 parts of urea, 2,465 parts of nitric acid (32 percent by weight) and 1,350 parts of water is reacted continuously in a three-stage cascade (consisting of 3 reactors each with a distillation column and reflux condenser) for 6 hours at from 125° to 133° C. During the reaction, 1,130 parts of 14.4 percent strength by weight nitric acid distill off. The reaction mixture is then diluted with a 3.5-fold volume of water whilst cooling and is neutralized to pH 3-4 with ammonia solution. The 2-methyl-4-nitroimidazole which separates out is centrifuged off, washed, dried and recrystallized from water. 1,060 parts of 2-methyl-4-nitroimidazole (81.5% of theory) of melting point 145°-146° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04145553 |
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| Source dataset | uspto-grants-1979_03 |
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| ORD ID | ord-84c908b3989c49cfb457a34d2f808d52 |
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| Source note | uspto-grants-1979_03 |
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