反応 #68132
ord-b3800d3d4a4d47b5aade6287fe2288ea
反応方程式
反応物
試薬
反応条件
後処理
- 1workup.ADDITIONwere added at room temperature
- 2温度refluxed
- 3温度with heating for 4 hours
- 4温度refluxed
- 5温度with heating for 4 hours
- 6温度refluxed
- 7温度with heating for 9.5 hours
- 8温度refluxed
- 9温度with heating for 1 hour
- 10温度refluxed
- 11温度with heating for 8 hours
- 12温度refluxed
- 13温度with heating for 6 hours
- 14その他the solvent was removed under reduced pressure
- 15workup.ADDITIONwas added
- 16その他The organic layer was separated
- 17抽出the aqueous layer was extracted with chloroform
- 18洗浄washed with aqueous saturated sodium chloride solution
- 19乾燥dried over anhydrous magnesium sulfate
- 20その他the solvent was removed under reduced pressure
- 21その他To the residue thus obtained
- 22ろ過the resulting solid was filtered
実験手順
To 1 mL of a 1,4-dioxane solution containing 30 mg of 4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)-1-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)cyclohexanecarbonitrile, 1 mL of 20% aqueous potassium hydroxide solution and 1 mL of ethanol were added at room temperature and refluxed with heating for 4 hours. Further, 1 mL of 20% aqueous potassium hydroxide solution was added and refluxed with heating for 4 hours, thereafter 1.5 mL of 20% aqueous potassium hydroxide solution was further added and refluxed with heating for 9.5 hours. After 1 mL of 20% aqueous potassium hydroxide solution and 0.5 mL of ethanol were added and refluxed with heating for 1 hour, further 1 mL of 20% aqueous potassium hydroxide solution was added and refluxed with heating for 8 hours. After 1 mL of 20% aqueous potassium hydroxide solution was added and refluxed with heating for 6 hours, the reaction mixture was cooled to the room temperature, the solvent was removed under reduced pressure. The residue was adjusted to pH 11 with 2.0 mol/L hydrochloric acid and chloroform was added. The organic layer was separated, and the aqueous layer was extracted with chloroform. The organic layer and extracts were combined, washed with aqueous saturated sodium chloride solution, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. To the residue thus obtained, diethyl ether was added, and the resulting solid was filtered to give 21 mg of 4-((2,3-dihydro-1,4-benzodioxin-6-ylmethyl)amino)-1-(2-(7-methoxy-4-methyl-2-oxoquinolin-1(2H)-yl)ethyl)cyclohexanecarboxamide as a white solid.