Lithium Hydroxide → HCID 57565215, 화합물

온도

40 °C

Compound from step 4 (22 mg, 0.041 mmol) was dissolved in 2 mL of THF/MeOH (3:1), followed by addition of 1N LiOH (5.0 eqv). The resulting mixture were stirred at 40° C. for 3 hours. The organic solvent was evaporated under N2 and residues were diluted with water (2 mL). The aqueous layers were partitioned with ether (2 mL). After removal of organic layers, the aqueous layers were neutralized by 1N HCl (5.0 eqv) and then extracted with ethyl acetate (5 mL). The organic layers were washed with H2O, brine, and dried over Na2SO4. The solution was concentrated in vacuo to afford {6-Methoxy-7-[4-(5-trifluoromethyl-pyridin-2-yl)-piperazine-1-sulfonyl]-benzo[b]thiophen-3-yl}-acetic acid. 1H NMR (400 MHz, CDCl3) δ 8.32 (s, 1H), 8.38 (s, 1H), 7.78 (d, 1H), 7.61 (d, 1H), 7.22 (s, 1H), 6.60 (m, 1H), 4.01 (s, 2H), 3.98 (s, 3H), 3.77 (m, 4H), 3.22 (m, 4H).

1. customThe organic solvent was evaporated under N2
2. additionresidues were diluted with water (2 mL)
3. customThe aqueous layers were partitioned with ether (2 mL)
4. customAfter removal of organic layers
5. extractionextracted with ethyl acetate (5 mL)
6. washThe organic layers were washed with H2O, brine
7. dry with materialdried over Na2SO4
8. concentrationThe solution was concentrated in vacuo

ORD 기록

ord-c46cadd0376a4d6592c7bfdda33ecef9

출처 데이터셋

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07834004B2