Potassium Carbonate → (3RS,4RS)-7-methoxymethyloxy-3-[4-(methoxymethyloxy)phenyl]-3-methyl-4-[4-(5-(4,4,5,5,5-pentafluoropentylsulfonyl)pentyloxy)phenyl]thiochroman

温度

100 °C

5-(5-Chloropentylsulfonyl)-1,1,1,2,2-pentafluoropentane (27 mg, 0.082 mmol), potassium carbonate (34 mg, 0.25 mmol) and 18-crown-6 (21 mg, 0.08 mmol) were added to benzene-dimethylformamide (1:1) solution (2 ml) of (3RS,4RS)-4-(4-hydroxyphenyl)-7-methoxymethyloxy-3-[4-(methoxymethyloxy)phenyl]-3-methylthiochroman (37 mg, 0.082 mmol) and then stirred for 8 hours at 100° C. under argon atmosphere. After adding water, the reaction solution was extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The crude product thus obtained was purified using silica gel plate (ethyl acetate:hexane=1:2) to obtain 41 mg (yield: 67%) of the title compound.

1. extractionthe reaction solution was extracted with ethyl acetate
2. washThe organic layer was washed with saturated saline
3. dry with materialdried over anhydrous magnesium sulfate
4. distillationdistilled under reduced pressure
5. customto remove the solvent
6. customThe crude product thus obtained
7. customwas purified

ORDレコード

ord-a4c262bb8eb34d24abf42c2a6b15d88e

出典データセット

uspto-grants-2000_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06153768