HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 59278130, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 59278225 | HCID 59278225 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ammonium Chloride | HCID 25517 | — |
| Product | HCID 59278130 | HCID 59278130 | — |
Reaction Steps
To a stirred solution of trifluoromethanesulfonic acid 4-((S)-1-{[1-(4-fluorophenyl)-1H-pyrazolo[3,4-c]pyridine-4-carbonyl]-amino}-propyl)-6-methanesulfonyl-pyridin-2-yl ester (0.08 g, 0.13 mmol) in DMF (2 mL) was added a 2.0 M solution of methylamine in THF (0.150 mL, 0.30 mmol) followed by DIPEA (0.05 mL, 0.3 mmol). After 16 hours, the mixture was diluted with saturated aqueous ammonium chloride (5 mL) and extracted with ethyl acetate (3×5 mL). The combined organic layers were dried over sodium sulfate and concentrated onto silica gel. The crude material was purified by silica gel chromatography eluting with a gradient of 0-100% ethyl acetate in hexanes to afford the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08063065B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-97476d8bdb1d48a48696b3699c2afeac |
| Source note | uspto-grants-2011_11 |