3'-Chloropropiophenone synthesis
- Product Name:3'-Chloropropiophenone
- CAS Number:34841-35-5
- Molecular formula:C9H9ClO
- Molecular Weight:168.62
Yield:34841-35-5 92.6%
Reaction Conditions:
Stage #1: ethyl bromidewith magnesium in tetrahydrofuran;Reflux;
Stage #2: 3-chloro-benzonitrile in tetrahydrofuran;
Stage #3: with hydrogenchloride in tetrahydrofuran;water;
Steps:
4
With the reflux condensation tube, dropping funnel of the magnesium powder is added into the reactor 48.0g (2.0 μM), tetrahydrofuran (THF) solution 400 ml, slowly added from the dropping funnel in the bromoethane 218.0g (2.0 μM), control of the reaction temperature 50 - 60 °C, the solution has been switch and the state, the completion of the dropping heating reflux 1.0 - 1.5h, magnesium reaction is complete, get the Grignard reagent. Under stirring, the chlorobenzonitrile between 275.2g (2.0 μM) slowly drop added to the above prepared Grignard reagent, after and milling, reaction 3.0 - 4.0h, to produce intermediate I, reaction finishes, does not need to separate, slowly dropping 3 mol/L hydrochloric acid hydrolysis of intermediate I, the branching off of the inorganic phase, the organic phase of the regular pressure distillation to remove the THF, reduced pressure distillation, get between chlorobenzene acetone.
References:
CN106699527,2017,A Location in patent:Paragraph 0019; 0024; 0025
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