2-Chloro-4-amino-6,7-dimethoxyquinazoline synthesis
- Product Name:2-Chloro-4-amino-6,7-dimethoxyquinazoline
- CAS Number:23680-84-4
- Molecular formula:C10H10ClN3O2
- Molecular Weight:239.66
157459-53-5
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Yield:23680-84-4 76%
Reaction Conditions:
with trichlorophosphate at 25 - 70; for 1 h;
Steps:
2
Example 2:2-chloro-4-amino-657-dimethoxyquinazoline:3,4-dimethoxy-6-cynoaniline-l-yl formamide (50 g, 0.326 mole) and phosphorous oxy chloride (500ml) is added in one lot at 25-3O0C. Then the reaction mixture is heated to 65- 7O0C for about one hour. After the completion of reaction, the reaction mixture is cooled to 25-3O0C. The reaction mixture is then poured over the cool water (5-60C) and stirred further for one hour. The product 2-chloro-4-amino-6,7-dimethoxyquinazolines, is filtered and suck dried. To the wet cake water (5 L) is added and the pH of the suspension was adjusted to 7.5- 8.0 using saturated aqueous sodium hydroxide solution. The product is filtered and the solid obtained is washed with water (5 L) followed by acetone (500 ml). The product is dried at 60-650C fox 24 hours. (41 gm, 76 %). HPLC purity is >99%. Melting Range: 276-2780CMass: [M+2]+ = 242.21H NMR (DMSO): delta 8 (2H,bs), 7.6 (lH,s), 7.1 (lH,s), 3.9-3.8 (6H,d).
References:
UNICHEM LABORATORIES LIMITED WO2008/84493, 2008, A2 Location in patent:Page/Page column 8
27631-29-4
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192869-38-8
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