反应详情

温度

60 °C

A mixture of (3-amino-5-chloro-pyridin-2-yl)-(2-chloro-phenyl)-methanone (26.8 mg. 0.10 mmol) and 3.4-dichloro-benzenesulfonyl chloride (24.5 mg, 0.10 mmol) in anhydrous pyridine (1 mL) were stirred overnight at 60° C. Reaction mixture was concentrated and the residue was treated with 1 M NaOH (5 mL) and THF(5 mL) to hydrolyze bis-sulfonamide. The resultant solution was neutralized to pH 6 and the aqueous layer was extracted with EtOAc. The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated. The was purified by preparative HPLC (20→90% gradient of MeCN-water) and pure product fractions were lyophilized to provide 3,4-dichloro-N[5-chloro-2-(2-chloro-benzoyl)-pyridin-3-yl]-benzenesulfonamide as a solid. MS m/z: 498.0 (M+Na).

1. customReaction mixture
2. concentrationwas concentrated
3. additionthe residue was treated with 1 M NaOH (5 mL) and THF(5 mL)
4. extractionthe aqueous layer was extracted with EtOAc
5. washThe combined organic extracts were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe was purified by preparative HPLC (20→90% gradient of MeCN-water) and pure product fractions