HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86677807, compound → HCID 86677808, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86677807 | HCID 86677807 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 86677808 | HCID 86677808 | 50% |
Reaction Steps
A solution of 3-{3-[1-(4-amino-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl]-5-chloro-6-cyano-2-methoxyphenyl}-N-(tert-butyl)azetidine-1-carboxamide (chiral intermediate from Example 292) (16 mg, 0.032 mmol) in trifluoroacetic acid (2 mL) was heated in the microwave at 120° C. for 10 min. The reaction mixture was diluted with methanol and purified by preparative LCMS (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.1% ammonium hydroxide, at flow rate of 60 mL/min) to give the desired product (7 mg, 50%). The product was isolated as a single enantiomer.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09199982B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-e2b1d8625cbb4840949c79a69e56e6d8 |
| Source note | uspto-grants-2015_12 |