ethyl 3-(2-chloropyridin-3-yl)-3-oxopropanoate synthesis
- Product Name:ethyl 3-(2-chloropyridin-3-yl)-3-oxopropanoate
- CAS Number:220731-02-2
- Molecular formula:C10H10ClNO3
- Molecular Weight:227.6443
Yield:220731-02-2 13.8 g
Reaction Conditions:
Stage #1: hydrogen ethyl malonatewith n-butyllithium in tetrahydrofuran at -78; for 1 h;
Stage #2: 2-Chloronicotinoyl chloride in tetrahydrofuran; for 3 h;
Steps:
1.2 Step 2: Preparation of 3-(2-chloropyridin-3-yl)-3-carbonylpropionic acid ethyl ester
3-ethoxy-3-carbonylpropionic acid (13.2 g, 100 mmol) was dissolved in tetrahydrofuran (100 mL), n-butyl lithium (25.6 g, 400 mmol) was added dropwise at -78° C., reacted at low temperature for 1 h, 2-chloronicotinoyl chloride (17.5 g, 99.4 mmol) in tetrahydrofuran (20 mL) solution was added, and continuously reacted at low temperature for 3 h. After reaction was complete, extraction was performed with water/dichloromethane, organic phase was rotated for dryness, and separated by column chromatography to obtain product 13.8 g.
References:
US9181244,2015,B1 Location in patent:Page/Page column 20; 21
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