HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 117728446, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | HCID 90003214 | HCID 90003214 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 117728446 | HCID 117728446 | 94.9% |
Reaction Steps
tert-Butyl 3-(4-amino-3-(2-fluoro-4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-1-yl)azetidine-1-carboxylate (800 mg) in TFA (8 mL) was stirred for 1 hour. To the residue was added EtOAc and 1 water and the layers were separated. The aqueous layer was extracted with EtOAc and the combined organic layer was evaporated to around 50 ml and washed with 2M HCl. The combined aqueous layer was adjusted with NaOH to pH 8-9, extracted with EtOAc and the combined organic layer washed with brine, and dried over Na2SO4. The solvent was removed to obtain 600 mg of 1-(azetidin-3-yl)-3-(2-fluoro-4-phenoxyphenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-amine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266895B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-e0ef154ca6e44a66b4de47200841ba6d |
| Source note | uspto-grants-2016_02 |