gamma-oxo-alpha-phenylbenzenebutyronitrile synthesis
- Product Name:gamma-oxo-alpha-phenylbenzenebutyronitrile
- CAS Number:6268-00-4
- Molecular formula:C16H13NO
- Molecular Weight:235.28
Yield:6268-00-4 97.8%
Reaction Conditions:
Stage #1: 2-hydroxy-2-methyl-propionitrilewith lithium hydroxide monohydrate in lithium hydroxide monohydrate;N,N-dimethyl-formamide at 20; for 0.5 h;
Stage #2: benzalacetophenone in lithium hydroxide monohydrate;N,N-dimethyl-formamide at 60;Temperature;
Steps:
1-14 Example 1 Synthesis of 4-oxo-2,4-diphenylbutyronitrile.
Add 18.4 mg of lithium hydroxide to a two-necked bottle equipped with a magnetic stirrer, add 1 ml of deionized water to the bottle, and ultrasonically vibrate to fully dissolve lithium hydroxide in water, and then add 2 ml of N,N-dimethylformamide to the bottle, at room temperature, keep the rotor rotating, add 0.106ml of acetone cyanohydrin, make it react for 30 minutes, then dissolve 100mg of chalcone in 2ml of N,N-dimethylformamide and add it to the reaction system, The reaction system was transferred to a constant temperature water bath at 60°C for continuous heating and stirring. The reaction was monitored by TLC. When the raw material disappeared, firstly add water for washing, add dichloromethane for extraction, then wash the organic phase with saturated brine and water, dry with anhydrous magnesium sulfate and concentrate to obtain the crude product. The crude product was subjected to flash column chromatography using n-hexane and 10% ethyl acetate as mobile phase column chromatography to obtain 4-oxo-2,3-diphenylbutyronitrile, 110.5 mg, white solid, yield 97.8 %.
References:
CN114456086,2022,A Location in patent:Paragraph 0018-0046; 0094
201230-82-2
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