Ethyl 3-(3-chloro-2,4,5-trifluorophenyl)-3-oxopropanoate → Ethyl 1-[3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridin-2-yl]-8-chloro-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylate

温度

90 °C

To 3 ml chloroform solution of ethyl 3-ethoxy-2-(3-chloro-2,4,5-trifluorobenzoyl)acrylate prepared from 0.84 g of ethyl 3-chloro-2,4,5-trifluorobenzoylacetate by normal process was added 0.75 g of 2-amino-3-fluoro-6-(1,1,3,3-tetramethylbutylamino)pyridine. The solution was concentrated under reduced pressure, and to the residue were added 0.65 g of anhydrous potassium carbonate and 1.5 ml of N,N-dimethylformamide, and the mixture was stirred at 90° C. for 1 hour and allowed to cool. The solution was separated by adding 30 ml of chloroform and 300 ml of distilled water, and the chloroform layer was washed twice with 300 ml of distilled water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The precipitate was collected by filtration and washed with ethanol and diisopropylether successively to obtain 0.45 g of the title compound as a pale yellow powder.

1. concentrationThe solution was concentrated under reduced pressure
2. additionto the residue were added 0.65 g of anhydrous potassium carbonate and 1.5 ml of N,N-dimethylformamide
3. temperatureto cool
4. customThe solution was separated
5. additionby adding 30 ml of chloroform and 300 ml of distilled water
6. washthe chloroform layer was washed twice with 300 ml of distilled water
7. dry with materialdried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. filtrationThe precipitate was collected by filtration
10. washwashed with ethanol and diisopropylether successively

ORDレコード

ord-0079c1db99c241a7bc31e8d14cec804e

出典データセット

uspto-grants-2000_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06156903