ChemicalBook CAS DataBase List 2-(chloromethyl)-4-methylquinazoline

2-(chloromethyl)-4-methylquinazoline synthesis

5synthesis methods

Product Name:2-(chloromethyl)-4-methylquinazoline
CAS Number:109113-72-6
Molecular formula:C10H9ClN2
Molecular Weight:192.64

Into a 500ml reaction flask, add o-aminoacetophenone, chloroacetonitrile, 1,4-dioxane, and N-methyl-3(3-sulfopropyl)imidazolium hydrogen sulfate prepared above. Stir to dissolve, cool the reaction system to 8°C, and dropwise add hydrochloric acid to the reaction system. The reaction temperature was kept unchanged during the dropwise addition. After that, the reaction was continued at 8°C for 18 hours to complete the reaction process. After the reaction, ammonia water (the concentration of ammonia water was 10wt%) at 5°C was added to the reaction system. After stirring and crystallizing at 5 for 30 minutes, filter to obtain a filter cake, washing the filter cake with water. Recrystallized with 200ml of dichloromethane to obtain 2-(chloromethyl)-4-methylquinazoline. yield: 85.14%

551-93-9 Synthesis

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79-07-2
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109113-72-6
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Yield:109113-72-6 94.26%

Reaction Conditions:

Stage #1: 2-aminoacetophenonewith phosphoric acid in ethanol at 20;
Stage #2: Chloroacetamide in ethanol;Reflux;Reagent/catalyst;Solvent;

Steps:

1-6 Example 1

Put 13.52g (0.1mol, M=135.17) of o-aminoacetophenone into the round bottom flask, Add 80ml of absolute ethanol and stir to dissolve, add 11.76g of catalyst H3PO4 (0.12mol, M=98), slowly add dropwise dissolved in 20ml absolute ethanol at room temperature A solution of 10.29g (0.11mol, M=93.51) of 2-chloroacetamide, after dripping, The reaction was refluxed for 45h, cooled and filtered, and the filtrate was washed with saturated brine, The solvent was evaporated and the organic phase was extracted with ethyl acetate and dried with anhydrous sodium sodium sulfate. Concentrate and dry in vacuo to obtain 18.16 g of solid intermediate II with a yield of 94.26%. The purity is 99.9%, and the maximum single impurity is 0.01%.

References:

CN112679500,2021,A Location in patent:Paragraph 0036-0048

551-93-9 Synthesis

551-93-9
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107-14-2 Synthesis