2,2-Difluoro-2-(fluorosulfonyl)acetic acid → methyl 3-[(2S)-1-(difluoromethoxy)propan-2-yl]oxy-5-phenylmethoxy-benzoate

温度

45 °C

2-(Fluorosulphonyl)difluoroacetic acid (0.239 mL, 2.31 mmol) was added dropwise, with stirring, to a degassed mixture of methyl 3-{[(1S)-2-hydroxy-1-methylethyl]oxy}-5-[(phenylmethyl)oxy]benzoate (0.73 g, 2.31 mmol) and copper (I) iodide (88 mg, 0.46 mmol) in acetonitrile (10 mL) at 45° C. The reaction was stirred at 45° C. for 24 hours. The solvent was removed in vacuo and ethyl acetate (30 mL) added. The organics were washed with water (30 mL), brine (30 mL), dried (MgSO4), filtered and the solvent removed in vacuo to give a yellow oil which was chromatographed on silica, eluting with a gradient of 0-30% ethyl acetate in isohexane, to give the desired compound (0.11 g).

1. customThe solvent was removed in vacuo and ethyl acetate (30 mL)
2. additionadded
3. washThe organics were washed with water (30 mL), brine (30 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customto give a yellow oil which
8. customwas chromatographed on silica
9. washeluting with a gradient of 0-30% ethyl acetate in isohexane

ORDレコード

ord-e2b57f3b921946a3b7fa9e518fa338b5

出典データセット

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07977328B2