Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | HCID 10192701 | HCID 10192701 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1-Methoxy-2-propanol | HCID 7900 | — |
| Product | HCID 44409760 | HCID 44409760 | 17.5% |
Reaction Steps
A mixture of cyclohexylamine (1.78 g, 18 mmol) and 6-chloro-N,2-dicyclopropyl-5-methyl-4-pyrimidinamine 33 (0.70 g, 3 mmol) in 1-methoxy-2-propanol (2 ml) is stirred at 125° C. for 120 hours. After cooling, the brown solution is diluted with dichloromethane, washed two times with a saturated sodium bicarbonate solution. The combined organic layers are dried over magnesium sulfate and concentrated under high vacuum to afford a brown oil. The crude oil is purified by column chromatography (dichloromethane/methanol: 97.3/2.7) to give pure N4-cyclohexyl-N6,2-dicyclopropyl-5-methyl-4,6-pyrimidinediamine 141 (0.150 g, 17%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07544675B2 |
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| Source dataset | uspto-grants-2009_06 |
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| ORD ID | ord-97128fb718a242888948861942551beb |
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| Source note | uspto-grants-2009_06 |
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