تفاعل #68132
ord-b3800d3d4a4d47b5aade6287fe2288ea
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1workup.ADDITIONwere added at room temperature
- 2درجة الحرارةrefluxed
- 3درجة الحرارةwith heating for 4 hours
- 4درجة الحرارةrefluxed
- 5درجة الحرارةwith heating for 4 hours
- 6درجة الحرارةrefluxed
- 7درجة الحرارةwith heating for 9.5 hours
- 8درجة الحرارةrefluxed
- 9درجة الحرارةwith heating for 1 hour
- 10درجة الحرارةrefluxed
- 11درجة الحرارةwith heating for 8 hours
- 12درجة الحرارةrefluxed
- 13درجة الحرارةwith heating for 6 hours
- 14أخرىthe solvent was removed under reduced pressure
- 15workup.ADDITIONwas added
- 16أخرىThe organic layer was separated
- 17استخلاصthe aqueous layer was extracted with chloroform
- 18غسيلwashed with aqueous saturated sodium chloride solution
- 19تجفيفdried over anhydrous magnesium sulfate
- 20أخرىthe solvent was removed under reduced pressure
- 21أخرىTo the residue thus obtained
- 22ترشيحthe resulting solid was filtered
الإجراء التجريبي
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.