HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(Ethoxycarbonylmethyl)-1H-pyrazole-4-boronic acid pinacol ester → 2-(4-{2-[2-(1-Methyl-piperidin-4-yl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-yl}-pyrazol-1-yl)-ethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(Ethoxycarbonylmethyl)-1H-pyrazole-4-boronic acid pinacol ester | HCID 16218385 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | 2-{4-[2-(2-Isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-yl]pyrazol-1-yl}-ethanol | HCID 56832510 | — |
| Reactant | 8-Bromo-2-[2-(1-methyl-piperidin-4-yl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene | HCID 58204111 | — |
| Product | 2-(4-{2-[2-(1-Methyl-piperidin-4-yl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-yl}-pyrazol-1-yl)-ethanol | HCID 58203719 | — |
Reaction Steps
Similarly to as described in General Procedure C: 8-Bromo-2-[2-(1-methyl-piperidin-4-yl)-2H-[1,2,4]triazol-3-yl]-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulene was reacted with ethyl 2-(4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazol-1-yl)acetate. The crude ester was reduced with lithium aluminum hydride as described for 2-{4-[2-(2-Isopropyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-3-thia-1-aza-benzo[e]azulen-8-yl]-pyrazol-1-yl}-ethanol. The product was purified by HPLC to give 303 as a colorless solid (27 mg). LCMS: 478.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08673952B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-7b71192c0c2e479798327914871bba0f |
| Source note | uspto-grants-2014_03 |