Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Carbonate Ion | HCID 19660 | — |
| Reactant | Ethanol hydrochloride | HCID 21887872 | — |
| Reactant | HCID 86706469 | HCID 86706469 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86706470 | HCID 86706470 | 80% |
Reaction Steps
Tert-butyl 3-(1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[3,4-d]pyrimidin-4-ylamino)azepane-1-carboxylate (0.5 g, 1.1 mmol) was dissolved conc HCl:EtOH (1:3, 10 mL) and the solution was heated to 60° C. for 4 h. The reaction mixture was concentrated in vacuo and the residue obtained was dissolved in MeOH and treated with solid supported carbonate resin to neutralize the solution. The reaction mixture stirred for 2 h and filtered off slurry, washed solid with MeOH (2×20 mL). The filtrate was concentrated in vacua to afford the titled intermediate (200 mg, 80%), which was used in the next step without further purification. LCMS: m/z [M+1]=233.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09273028B2 |
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| Source dataset | uspto-grants-2016_03 |
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| ORD ID | ord-3bce2d5950074fd49037f0e286698e1a |
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| Source note | uspto-grants-2016_03 |
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