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17336-90-2

3,4-Dimethyl-2(1H)-quinolinone synthesis

7synthesis methods
32315-10-9 Synthesis
Triphosgene

32315-10-9
433 suppliers
$10.00/1g

133901-59-4 Synthesis
(E)-2-(But-2-en-2-yl)aniline

133901-59-4
3 suppliers
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3,4-Dimethyl-2(1H)-quinolinone

17336-90-2
2 suppliers
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Yield:17336-90-2 86%

Reaction Conditions:

with triethylamine in dichloromethane at 60; for 12 h;Inert atmosphere;Glovebox;Schlenk technique;

Steps:

General Procedure of Products (2).

General procedure: An oven-dried Schlenk tube (25 mL) containing a stirring bar was charged with the substrate (0.3 mmol). The Schlenk tube was then introduced in a glovebox where it was charged with triphosgene (44.5 mg, 0.15 mmol, 0.5 equiv.). The tube was taken out of the glovebox and connected to a vacuum line where it was evacuated and back-filled under N2 flow for at least 3 times. The DCM (5 mL) and Et3N (0.3 mmol, 1 equiv.) were added under N2 flow. Once added, the tube was closed at atmospheric pressure of N2 (1 atm) and stirred for 12 h at 60 °C. Then, the mixture was cooled to room temperature, quenched with 2 mL water, then concentrated in vacuo. The residue was purified by silica gel flash chromatography (petroleum ether/AcOEt 3/1) to give the pure target product 2. (the procedure of control experiments and the reaction in lager scale are similar.)

References:

Du, Guizhi;Wang, Zixiao;Zhang, Zhen [Heterocycles,2020,vol. 100,# 4,p. 600 - 608]