Ethyl 2-Cyano-3-methoxy-3-phenylprop-2-enoate synthesis
- Product Name:Ethyl 2-Cyano-3-methoxy-3-phenylprop-2-enoate
- CAS Number:70638-61-8
- Molecular formula:C13H13NO3
- Molecular Weight:231.25
Yield:-
Reaction Conditions:
Stage #1: ethyl (E/Z)-2-cyano-3-hydroxy-3-phenylacrylatewith sodium hydroxide at 0 - 5; for 0.166667 h;
Stage #2: dimethyl sulfate at 0.5; for 4 h;Reagent/catalyst;Temperature;
Steps:
1-2 Example 1:
Put 114 g of ethyl cyanoacetate (1 mol, 99%), 60.6 g of sodium hydroxide (1.5 mol, 99%), and 300 g of 99% ethanol into a reaction flask. 185 g (1.3 moles, 99%) of acid chloride was dripped in about an hour. After dripping, it was kept at 10-15 °C for 2 hours. After the reaction was completed, the reaction solution of intermediate (III) was obtained, and then 44.44% of sodium hydroxide was added. g (1.1 moles, 99%), The internal temperature was lowered to 05°C, and after the temperature was stable for 10 minutes, 152.7 g (1.2 mol, 99%) of dimethyl sulfate was added dropwise, and the dropping was completed within 1 hour, and the reaction was carried out at 05°C for 3 hours. Obtain the reaction solution of intermediate (IV), raise the temperature to 3540 , feed 25.5 grams of ammonia gas in 0.51 hour, keep warm for half an hour, steam ethanol, add 100 grams of water, Compound (V) 2-cyano-3-amino ethyl acrylate was precipitated, filtered, and dried to obtain 105 g, with a content of 96%.
References:
CN113845443,2021,A Location in patent:Paragraph 0016; 0032; 0036
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