4-ethoxy-3-(ethoxycarbonyl)-4-oxobut-2-enoic acid synthesis
- Product Name:4-ethoxy-3-(ethoxycarbonyl)-4-oxobut-2-enoic acid
- CAS Number:431911-73-8
- Molecular formula:C9H12O6
- Molecular Weight:216.19
188973-69-5
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Yield:431911-73-8 73%
Reaction Conditions:
with trifluoroacetic acid in dichloromethane at 0 - 25; for 45 h;
Steps:
β, β-Dibenzoyl acrylic acid (4a)
General procedure: To a solution of 3a (2.28 g, 6.78 mmol) in CH2Cl2 (3 ml) at 0 °C was added CF3COOH (3 ml) dropwise. The resulting mixture was warmed to 25 °C and stirred for 45 h before it was diluted with CH2Cl2 (50 ml), and washed with water (20 ml). The organic layer was separated, the aqueous layer was extracted with CH2Cl2 (3*40 ml). The combined organic layers were washed with bine (20 ml), dried (Na2SO4), and concentrated in vacuo. Flash column chromatography (silica gel, petroleum ether:EtOAc 5: 1, 3: 1, 2: 1) afforded 4a as colorless oil (1.63 g, 86%).
References:
Yu, Qunying;Yu, Jingmou;Bao, Haiou;Hu, Xiao;Ying, Danxia;Wu, Lixia;Liu, Fang;Jiang, Honghong;Jinxia, Zhong;Zhang, Shuihua [Synthetic Communications,2018,vol. 48,# 15,p. 1939 - 1944] Location in patent:supporting information
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609-09-6
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61063-74-9
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431911-73-8
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