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ChemicalBook CAS DataBase List 4,7-Dichloroquinazoline
2148-57-4

4,7-Dichloroquinazoline synthesis

5synthesis methods
7-CHLORO-4-QUINAZOLINOL

31374-18-2

4,7-Dichloroquinazoline

2148-57-4

The general procedure for the synthesis of 4,7-dichloroquinazoline from 7-chloro-4(3H)-quinazolinone was as follows: 7-chloro-3H-quinazolin-4-one (170, 0.155 g, 0.85830 mmol) was dissolved in a screw cap vial containing 1 mL of phosphorus oxychloride (POCl3). After sealing the vial, the reaction was placed in an oil bath at 100 °C for 3 hours. Upon completion of the reaction, the resulting solution was concentrated under vacuum and distilled three times by azeotropic distillation with toluene to completely remove the residual phosphorous trichloride, resulting in the target compound 4,7-dichloroquinazoline (171, 0.162 g, 0.81391 mmol, 94.828% yield). The mass spectrometry analysis showed m/z 199.0 ([M+H]+).

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Yield:2148-57-4 94.828%

Reaction Conditions:

with trichlorophosphate at 100; for 3 h;

Steps:

11.1 Example 11 Step 1 - synthesis of 4,7-dichloroquinazoline (171)
7-Chloro-3H- quinazolin-4-one (170, 0.155 g, 0.85830 mmol) was dissolved in 1 mL of POCI3 in a screw cap vial. The vial was sealed and placed in a 100 °C oil bath for 3 hours. The resulting solution was concentrated under vacuum and co-concentrated from toluene three times to provide the desired compound (171, 0.162 g, 0.81391 mmol, 94.828%). MS: 199.0 m/z (M+H)+.

References:

ELAN PHARMACEUTICALS, INC.;XU, Ying-Zi;ARTIS, Dean, R.;BOWERS, Simeon;HOM, Roy, K.;SHAM, Hing, L.;YUAN, Shendong WO2013/142613, 2013, A1 Location in patent:Page/Page column 175

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