7-methoxy-3,4-dihydro-1-naphthalenylacetonitrile synthesis
- Product Name:7-methoxy-3,4-dihydro-1-naphthalenylacetonitrile
- CAS Number:861960-34-1
- Molecular formula:C13H13NO
- Molecular Weight:199.25
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Yield:861960-34-1 96.3%
Reaction Conditions:
with oenanthic acid;benzylamine in toluene at 140; for 48 h;
Steps:
1 Step 1) Preparation of 2- (7-methoxy-3,4-dihydro-1-yl) acetonitrile
The mixture of 7-methoxy-3,4-dihydro-naphthalene -1 (2H) - one (5.00g, 28.37mmol), 2-cyanoacetic acid (3.62g, 42.56mmol), heptanoic acid (1.0mg, 7.09 mmol) and benzylamine (0.78mL, 7.09mmol) in toluene (30 mL), and the reaction in an oil bath at 140° 48h, the reaction was stopped, cooled to 25° . Washed with saturated sodium bicarbonate solution (100 mL) and saturated brine (40 mL) After washing, liquid separation the organic phase was dried over anhydrous sodium sulfate. Filtered and the filtrate under reduced pressure to spin dry, and purified by column chromatography (petroleum ether / ethyl acetate (v / v) = 50/1) to give a yellow solid (5.44g, 96.3%) of the title compound.
References:
CN104292125,2016,B Location in patent:Paragraph 0229; 0230; 0231; 0232
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