Triphenylphosphine → 3-Chloro-4-[(6-methylpyridin-2-yl)methoxy]aniline

To a mixture of (6-methyl-pyridin-2-yl)-methanol (280 mg, 2.29 mmol), 4-amino-2-chloro-phenol (359 mg, 2.5 mmol) and triphenylphosphine (0.655 mg, 2.5 mmol) in THF (8 ml) was added DIAD (0.49 ml, 2.5 mmol) and the mixture was stirred at rt for 20 h. The mixture was concentrated in vacuo, diluted with 1N HCl (30 ml), washed with EtOAc (3×20 ml) and basified to pH 12 by 1N NaOH. The mixture was extracted with EtOAc (4×40 ml); the combined EtOAc extracts were washed with brine (1×20 ml), dried (MgSO4), filtered and concentrated in vacuo to give 15A (?? mg, ??% pure)

1. concentrationThe mixture was concentrated in vacuo
2. additiondiluted with 1N HCl (30 ml)
3. washwashed with EtOAc (3×20 ml)
4. extractionThe mixture was extracted with EtOAc (4×40 ml)
5. washthe combined EtOAc extracts were washed with brine (1×20 ml)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo

ORDレコード

ord-b298dfc11e964586aa31546be83e2eb2

出典データセット

uspto-grants-2006_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07064203B2