1-Chloromethyl naphthalene synthesis
- Product Name:1-Chloromethyl naphthalene
- CAS Number:86-52-2
- Molecular formula:C11H9Cl
- Molecular Weight:176.64
Yield:86-52-2 97.1%
Reaction Conditions:
with hydrogenchloride;ferric(III) chloride;benzyl-triethyl-ammonium chloride;copper chloride (II) in lithium hydroxide monohydrate at 40; for 3 h;Temperature;
Steps:
1.a; 1.b; 2.a; 2.b; 3.a; 3.b; 4.a; 4.b; 5.a; 5.b; 6.a; 6.b; 1-2
In step a, 128g (1mol) of naphthalene, 60g (2mol) of paraformaldehyde, 3.25g (0.02mol) of FeCl, 2.69g (0.02mol) of CuCl2, 3.42g (0.015mol) of benzyltriethylammonium chloride and the mass of 214.7 g (2.5 mol) of hydrochloric acid solution with a concentration of 42.5% were mixed evenly, the temperature was raised to 40°C and the reaction was maintained for 3 h, the temperature was lowered, and the solution was left to stand for separation. The oil phase was washed twice with 10wt% potassium carbonate solution and water to obtain 1-chlorine Crude methylnaphthalene;In step b, the crude 1-chloromethylnaphthalene was added to 192 g of absolute ethanol, heated to 26 °C to dissolve, then cooled to -5 °C at a rate of 0.5 °C/10min for 2 hours, then filtered and washed with absolute ethanol. , the filter cake was placed in a vacuum drying oven, and dried at 25 mmHg and 35° C. for 5 h to obtain 171.5 g of 1-chloromethylnaphthalene product with a content of 99.6% and a yield of 97.1%.
References:
CN113999086,2022,A Location in patent:Paragraph 0040-0072
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