反应详情

19.6 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added under ice cooling to a 200 mL tetrahydrofuran solution of 19.9 g of the compound obtained in step 2-2 and 17.3 g of 1-hydroxybenzotriazole monohydrate, and the reaction mixture was stirred for 30 minutes at the same temperature. After this, 9.24 g of a 50% dimethylamine aqueous solution was added to the reaction solution, and the reaction mixture was stirred for 1 hour while the temperature was raised to room temperature. 150 mL of solvent was distilled off under reduced pressure, and to the residue thus obtained was added 100 mL of chloroform and 100 mL of a 10% potassium carbonate aqueous solution. After liquid separation, the aqueous layer was extracted with chloroform, and the combined organic layer was washed with saturated brine and then dried with magnesium sulfate, after which the drying agent was filtered off and 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 20.5 g of the titled compound (colorless solid).

1. stirringthe reaction mixture was stirred for 1 hour while the temperature
2. distillation150 mL of solvent was distilled off under reduced pressure
3. customto the residue thus obtained
4. customAfter liquid separation
5. extractionthe aqueous layer was extracted with chloroform
6. washthe combined organic layer was washed with saturated brine
7. dry with materialdried with magnesium sulfate
8. filtrationafter which the drying agent was filtered off
9. distillationthe solvent was distilled off under reduced pressure
10. customThe residue thus obtained