(E)-2-(7-methoxy-3,4-dihydronaphthalen-1(2H)-ylidene)acetonitrile synthesis
- Product Name:(E)-2-(7-methoxy-3,4-dihydronaphthalen-1(2H)-ylidene)acetonitrile
- CAS Number:127299-26-7
- Molecular formula:C13H13NO
- Molecular Weight:199.25
Yield:127299-26-7 100%
Reaction Conditions:
with sodium methylate in methanol at -20 - -10; for 24 h;Wittig Rearrangement;Reagent/catalyst;
Steps:
1 Example 1 Preparation of (7-methoxy-3,4-dihydro-2H-naphthalene-1-ylidene) acetonitrile
The reaction flask was charged with 100 g of 7-methoxy-1-naphthalenone, 153.2 g of 30% sodium methoxide, 400 ml of methanol,Stirring, temperature -20 ~ -10 , dropping 140.7g diethyl cyanomethyl phosphate, drop Bi,Maintain the temperature -20 ~ -10 reaction for about 24h.TLC detection reaction is complete, the reaction solution by adding hydrochloric acid to pH = 7, evaporated under reduced pressure,700 ml of dichloromethane and 700 ml of water were added to the mixture, and the layers were separated by standing, and the dichloromethane layer and the aqueous layer were separated.The aqueous layer was washed with 200 ml of dichloromethane and the washings were combined with the dichloromethane layer and then washed with 200 ml of water.The washed dichloromethane layer was evaporated under reduced pressure,(7-methoxy-3,4-dihydro-2H-naphthalene-1-ylidene) acetonitrile in a yield of 100%Purity (trans and cis) greater than 98%
References:
CN104803882,2017,B Location in patent:Paragraph 0063; 0064; 0065; 0066; 0067; 0068
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