Sodium methanesulfinate → HCID 67341497、化合物

温度

90 °C

Methanesulphinic acid sodium salt (748 mg, 7.33 mmol) was added to (3-bromo-5-fluorophenyl)methanol (501 mg, 2.44 mmol) and copper(I) iodide (0.248 mL, 7.33 mmol) in DMSO (12 mL) under nitrogen. The resulting mixture was stirred at 90° C. for 3 days. The reaction mixture was diluted with EtOAc (300 mL), then filtered. The filtrate was washed sequentially with water (200 mL) and saturated brine (2×200 mL). The organic layer was dried over Na2SO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 70 to 100% EtOAc in isohexane. Pure fractions were evaporated to dryness to afford [3-fluoro-5-(methylsulfonyl)phenyl]methanol (240 mg, 48.1%) as a white solid.

1. filtrationfiltered
2. washThe filtrate was washed sequentially with water (200 mL) and saturated brine (2×200 mL)
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. customevaporated
6. customto afford crude product
7. customThe crude product was purified by flash silica chromatography, elution gradient 70 to 100% EtOAc in isohexane
8. customPure fractions were evaporated to dryness

ORDレコード

ord-efdbf89e5d3d48bda33a352e1fa21338

出典データセット

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08003649B2