Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 178493095 | HCID 178493095 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 178493097 | HCID 178493097 | — |
Reaction Steps
A mixture of 5,6-dichloro-N2-[(1S)-1-(5-fluoropyrimidin-2-yl)ethyl]-N4-(5-methoxy-1H-pyrazol-3-yl)pyrimidine-2,4-diamine (Example 30, 100 mg), morpholine (0.026 mL) and DIPEA (0.066 ml) in n-BuOH (2.0 ml) was charged into a microwave reaction vessel. The vessel was sealed and heated at 150° C. for 24 hours. The solvent was removed under reduced pressure and the residue was purified by Gilson 2%-40% MeCN/H2O, 15 minutes) to give the titled compound as solid (21.8 mg). 1H NMR δ 11.99 (s, 1H) 9.30 (s, 1H) 8.82 (s, 2H) 7.89 (d, 1H) 5.49 (s, 1H) 4.93-5.14 (m, 1H) 3.75 (s, 3H) 3.44-3.62 (m, 4H) 3.09-3.27 (m, 4H) 1.47 (d, 3H) m/z 450.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08088784B2 |
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| Source dataset | uspto-grants-2012_01 |
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| ORD ID | ord-8e240b4834f54134874f9f43f88ee403 |
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| Source note | uspto-grants-2012_01 |
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