Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | 2,4,6-Trichloropyrimidine | HCID 77378 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 20359978 | HCID 20359978 | — |
Reaction Steps
A solution of 151.5 g (1 mol) of 2,4,6-trichloropyrimidine in 300 ml of acetonitrile is taken and 285 g (5 mols) of cyclopropylamine are added dropwise at 20°-30°, whilst cooling. The solution is warmed to 40° for 5 hours and to 70° for about 12 hours. The suspension is concentrated to dryness on a rotary evaporator and the residue is thoroughly stirred with 1,500 ml of methylene chloride and 1,000 ml of water for 30 minutes. The undissolved constituent is filtered off on a cloth filter. It consists of practically pure 4,6-di-cyclopropylamino-2-chloropyrimidine. The phases of the filtrate are separated and the organic phase is again extracted with water, dried and concentrated to give an oil. This is distilled under a high vacuum (boiling point 149°-51°/0.1 mm) and is then recrystallised from methanol, with addition of water. The colourless product has a melting point of 58°-60°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04082535 |
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| Source dataset | uspto-grants-1978_04 |
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| ORD ID | ord-792e6bd9e6fd4a599dbb998ed6898f6a |
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| Source note | uspto-grants-1978_04 |
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