反应详情

A 40 mL tetrahydrofuran solution of 4.00 g of the compound obtained in step 3-3 and 3.23 g of 1-hydroxybenzotriazole monohydrate was stirred for 30 minutes under ice cooling. 3.66 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was then added, and the reaction mixture was stirred for 30 minutes at the same temperature. 2.15 g of a 50% dimethylamine aqueous solution was added to the reaction solution, after which the reaction mixture was stirred for 1 hour at room temperature. 60 mL of chloroform and 50 mL of a 5% potassium carbonate aqueous solution were added to the reaction solution, liquid separation was performed, the aqueous layer was extracted with chloroform (50 mL×2), the combined organic layer was washed with 30 mL of saturated brine and then dried with magnesium sulfate, and the drying agent was filtered off, after which the solvent was distilled off under reduced pressure. The residue thus obtained was subjected to column chromatography (silica gel 60, mobile phase: ethyl acetate/n-hexane=1/1 to 10/0; v/v) to obtain 4.02 g of the titled compound (colorless solid).

1. stirringafter which the reaction mixture was stirred for 1 hour at room temperature
2. extractionthe aqueous layer was extracted with chloroform (50 mL×2)
3. washthe combined organic layer was washed with 30 mL of saturated brine
4. dry with materialdried with magnesium sulfate
5. filtrationthe drying agent was filtered off
6. distillationafter which the solvent was distilled off under reduced pressure
7. customThe residue thus obtained