Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 18789072 | HCID 18789072 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 18789136 | HCID 18789136 | 44.6% |
Reaction Steps
In 18 ml of anhydrous dimethylformamide were dissolved 1.75 g (6.36 mmol) of 7-chloro-6-(2-chloroethyl)-5-methyl-3-nitropyrazolo[1,5-a]pyrimidine, and 0.93 g (12.72 mmol) of tert-butylamine and 1.61 g (15.94 mmol) of triethylamine were successively added to the solution, and the mixture was stirred at room temperature for 6 hours. Thereafter, the reaction mixture was poured into water and extracted with ethyl acetate (150 ml×2). The ethyl acetate layers were put together, washed with a saturated saline solution and dried over anhydrous magnesium sulfate, and the solvent was then distilled off. The residue was subjected to column chromatography on silica gel (hexane:ethyl acetate=2:1) and recrystallized from ethanol to obtain 0.78 g (yield: 44.6%) of the intended product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06057330 |
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| Source dataset | uspto-grants-2000_05 |
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| ORD ID | ord-ccb86954371f4ff1a55ea60a7ab0285b |
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| Source note | uspto-grants-2000_05 |
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