反应详情

温度

50 °C

351 mg of methyl 4-{[(6-{(2-fluoropropyl)[(4-methyl-1,3-thiazol-2-yl)sulfonyl]amino}-2,3-dihydro-1H-inden-5-yl)oxy]methyl}benzoate was dissolved in 5.00 mL of THF and 5.00 mL of methanol, and 2.03 mL of a 1 M aqueous sodium hydroxide solution was added thereto, followed by stirring at 50° C. for 4 hours. The reaction liquid was concentrated under reduced pressure, to the obtained residue were added a 5% w/v aqueous citric acid solution and chloroform, and the organic layer was separated using a Phase Separate-filter manufactured by Isotute, and dried over anhydrous sodium sulfate. The solvent was evaporated and the obtained residue was dissolved in 5.00 mL of ethanol, and 0.765 mL of an aqueous sodium hydroxide solution was added thereto, followed by concentration under reduced pressure. The obtained crude product was crystallized by the addition of isopropanol/ethanol, collected by filtration, and dried under reduced pressure to obtain 268 mg of sodium 4-{[(6-{(2-fluoropropyl)[(4-methyl-1,3-thiazol-2-yl)sulfonyl]amino}-2,3-dihydro-1H-inden-5-yl)oxy]methyl}benzoate.

1. customThe reaction liquid
2. concentrationwas concentrated under reduced pressure, to the obtained residue
3. additionwere added a 5% w/v aqueous citric acid solution and chloroform
4. customthe organic layer was separated
5. filtrationSeparate-filter
6. dry with materialdried over anhydrous sodium sulfate
7. customThe solvent was evaporated
8. dissolutionthe obtained residue was dissolved in 5.00 mL of ethanol
9. addition0.765 mL of an aqueous sodium hydroxide solution was added
10. concentrationfollowed by concentration under reduced pressure
11. customThe obtained crude product
12. customwas crystallized by the addition of isopropanol/ethanol
13. filtrationcollected by filtration
14. customdried under reduced pressure