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557770-90-8

7-(3-CHLOROPROPOXY)-4-CHLOROQUINAZOLINE synthesis

3synthesis methods
-

Yield:557770-90-8 91.23%

Reaction Conditions:

with thionyl chloride;N,N-dimethyl-formamide at 80; for 2 h;

Steps:

1.3 Step 3: 4-chloro-7-(3-chloropropoxy)quinazoline

7-(3-hydroxypropoxy)quinazolin-4(3H)-one (2.60g, 11.81mmol) was dissolved in thionyl chloride (25mL), Add anhydrous DMF (0.3 mL),The temperature was raised to 80 ° C for 2 hours. The reaction was stopped, cooled to room temperature, and the remaining thionyl chloride was evaporated under reduced pressure. dichloromethane (100 mL) was added to the mixture, and saturated sodium bicarbonate (100 mL) was washed once, and brine (50 mL) was washed once.Dry anhydrous sodium sulfate (50 g) was dried. The solvent was removed and the residue was dissolved in ethyl-t-butyl ether (30mL).Filter to remove insoluble matter,The filtrate was evaporated to dryness to give a white solid (2.76g, 91.23%).

References:

CN104098551,2019,B Location in patent:Paragraph 0238; 0245-0247

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