Methanol → Methyl 3-fluoro-2-hydroxybenzoate

温度

40 °C

To a solution of 3-fluoro-2-hydroxy-benzoic acid (5.0 g, 32 mmol) in methanol (20 mL) was added thionyl chloride (5.0 g, 42 mmol) dropwise and the reaction mixture was stirred at 40° C. for 3 hours, then heated at 50° C. for 16 hours. The reaction mixture was cooled and concentrated in vacuo and resulting residue was purified by silica gel column chromatography using 0-50% ethyl acetate/hexanes mixtures as eluant to give methyl 3-fluoro-2-hydroxy-benzoate (5.1 g, 94%) as white crystals. ESI-MS m/z calc. 170.0. Found 170.9 (M+1)+; Retention time: 1.33 minutes (3 min run).

1. temperatureheated at 50° C. for 16 hours
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated in vacuo
4. customresulting residue
5. customwas purified by silica gel column chromatography

ORDレコード

ord-69bec4cc329b42299e5d64fc6c767f2f

出典データセット

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08828996B2