HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 57968878, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | HCID 57969151 | HCID 57969151 | — |
| Reactant | HCID 86636439 | HCID 86636439 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 57968878 | HCID 57968878 | 29% |
Reaction Steps
To a clear solution of mixture of 9 and 10 (6-[2-(tert-butyl-dimethyl-silanyloxy)-ethylamino]-2-[3-formyl-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-phenoxy]-nicotinonitrile and 6-[2-(tert-butyl-dimethyl-silanyloxy)-ethylamino]-2-(3-formyl-phenoxy)-nicotinonitrile) in MeOH (anhydrous, 200 mL) was slowly added NaBH4 (0.26 g, 6.9 mmol). The reaction was stirred at room temperature for 4 hours, before the addition of HCl solution (1 M, 30 mL). After overnight at room temperature, the solution was slowly evaporated in vacuo. Purification was accomplished by reverse phase Biotage with 5%-100% MeOH/H2O gradient to afford 120 mg (29% yield) of the title compound as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09416146B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-01137e6d16ca45679745b23229d9d2b7 |
| Source note | uspto-grants-2016_08 |