Water → 3-(2,4-Dichloro-phenyl)-1,1,1-trifluoro-2-[2-(2-hydroxy-ethoxy)-pyridin-4-yl]-butan-2-ol

温度

45 °C

{4-[2-(2,4-Dichloro-phenyl)-1-hydroxy-1-trifluoromethyl-propyl]-pyridin-2-yloxy}-acetic acid methyl ester (Example 120, 70 mg) was dissolved in THF (5 mL) and treated with LiBH4 (10 mg). After 2 h stirring at 45° C. another portion of LiBH4 (5 mg) was added and the reaction mixture further stirred at 45° C. for 2 h. After cooling down to r.t., 3 drops of 1N aqueous HCl were added, followed by water (5 mL). The reaction mixture was then extracted twice with ethyl acetate. The combined organic phases were washed with brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by flash chromatography (10 g silica gel, ethyl acetate/heptane 30:70) to give the title compound as colorless foam (52 mg). MS (m/e)=410.3 (MH+).

1. additionwas added
2. temperatureAfter cooling down to r.t.
3. extractionThe reaction mixture was then extracted twice with ethyl acetate
4. washThe combined organic phases were washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography (10 g silica gel, ethyl acetate/heptane 30:70)

ORDレコード

ord-a8bf3e9e7d084056b3bdaf9cf296abdc

出典データセット

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08883786B2