HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 71522919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | 2,2-Difluoro-2-(fluorosulfonyl)acetic acid | HCID 2737516 | — |
| Reactant | HCID 178516074 | HCID 178516074 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 71522919 | HCID 71522919 | 41.8% |
Reaction Steps
2,2-Difluoro-2-(fluorosulfonyl)acetic acid (9.72 mg, 0.054 mmol, 1 eq) is added slowly, under stirring, to a mixture of 1-(3-{2-[3-(6-hydroxypyridin-2-yl)pyrrolidin-1-yl]ethyl}pyridin-2-yl)piperidin-2-one a16-1 (20 mg, 0.054 mmol, 1 eq) and dry sodium sulfate (0.78 mg, 0.005 mmol, 0.1 eq) in dry acetonitrile (400 μl). The reaction is stirred for 2 h at room temperature, then water (100 μl) is added. The resulting solution is concentrated in vacuo. The residue is purified by basic reverse phase chromatography (gradient: H2O/acetonitrile/NH4OH from 50/50/0.1 to 20/80/0.1) to afford 9.4 mg of 1-[3-(2-{3-[6-(difluoromethoxy)pyridin-2-yl]pyrrolidin-1-yl}ethyl)pyridin-2-yl]piperidin-2-one 109.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09067930B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-30df3278c29c4c0ca038af2df56b2477 |
| Source note | uspto-grants-2015_06 |