Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylamine tetrahydrofuran | HCID 22320367 | — |
| Reactant | HCID 86721466 | HCID 86721466 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86721468 | HCID 86721468 | 87.3% |
Reaction Steps
[step 6] (E)-2-{8-[(8-chloro-2-cyclopropylimidazo[1,2-a]pyrazin-3-yl)methyl]-3-fluorodibenzo[b,e]oxepin-11(6H)-ylidene}propanenitrile (0.2 g, 0.43 mmol) obtained in step 5 was dissolved in THF (1.4 mL), and 2 mol/L dimethylamine THF solution (1.7 mL, 3.4 mmol) was added. The mixture was stirred with heating at 100° C. for 1.5 hr in an Emrys Optimizer microwave synthesizer. Water was added to the mixture, and the mixture was extracted 3 times with ethyl acetate. The combined organic layers were dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (heptane/ethyl acetate=100/0 v/v-50/50 v/v) to give the title compound (0.18 g, 87%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08969345B2 |
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| Source dataset | uspto-grants-2015_03 |
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| ORD ID | ord-51c6d43f9845496abcaf272d1c216879 |
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| Source note | uspto-grants-2015_03 |
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