Hydrochloric Acid → 5-fluoro-1-(2-fluoro-phenyl)-3-(1-methyl-piperidin-3-ylmethoxy)-1H-indazole hydrogen chloride

To a room temperature stirred solution of Intermediate 57 (0.127 g, 0.278 mmol) in EtOAc (0.925 ml) was added 0.902 ml of a 4.0 M HCl solution in dioxane. The reaction was allowed to stir overnight at room temperature. Upon completion as indicated by HPLC, the reaction was concentrated under reduced pressure. EtOAc was added to the solid and then concentrated down under reduced pressure. This process was repeated five times. The solid was triturated with EtOAc/Et2O (2:1), the solid was filtered and then washed with Et2O (2×15 ml). The solid was placed in a drying oven under reduced pressure to yield 0.089 g (81.7%) of the title product.

1. concentrationthe reaction was concentrated under reduced pressure
2. additionEtOAc was added to the solid
3. concentrationconcentrated down under reduced pressure
4. customThe solid was triturated with EtOAc/Et2O (2:1)
5. filtrationthe solid was filtered
6. washwashed with Et2O (2×15 ml)
7. customThe solid was placed in a drying oven under reduced pressure

ORD 기록

ord-4d3942872b814869a0990daf77a1908c

출처 데이터셋

uspto-grants-2008_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07423054B2