Potassium Carbonate → Ethyl 1-(2-acetoxyethyl)-6-(2,3-dichlorobenzyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylate

温度

80 °C

Ethyl 6-(2,3-dichlorobenzyl)-1,4-dihydro-4-oxo-3-quinolinecarboxylate (400 mg, 1.1 mmol) obtained in Step 3 was suspended in dimethylformamide (DMF; 8 ml), 2-bromoethyl acetate (152 μl, 1.4 mmol) and potassium carbonate (440 mg, 3.2 mmol) were added, and the mixture was stirred with heating at 80° C. 2-Bromoethyl acetate (152 μl, 1.4 mmol) was added twice on the way, and the mixture was stirred with heating at 80° C. for 1.5 hr in total. After allowing to cool, saturated aqueous ammonium chloride was added to the reaction mixture, and the precipitated solid was collected by filtration, washed with water, and vacuum dried to give the object product (468 mg, yield 95%) as a white solid.

1. stirringthe mixture was stirred
2. temperaturewith heating at 80° C. for 1.5 hr in total
3. temperatureto cool
4. filtrationthe precipitated solid was collected by filtration
5. washwashed with water, and vacuum
6. customdried

ORDレコード

ord-4915396e966b4f0bb34f8fe36b0da60d

出典データセット

uspto-grants-2009_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07531554B2