4-chloro-2,5-dimethylquinazoline synthesis
- Product Name:4-chloro-2,5-dimethylquinazoline
- CAS Number:147006-57-3
- Molecular formula:C10H9ClN2
- Molecular Weight:192.64
147006-56-2
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147006-57-3
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Yield:147006-57-3 58.61%
Reaction Conditions:
with triethylamine;trichlorophosphate at 0; for 3 h;
Steps:
3 Step 3: synthesis of 4-chloro-2, 5-dimethylguinazoline 40
Triethyl amine (5.05 g, 49.9 mmol) was added to a mixture of intermediate 40-c(2.90 g, 16.7 mmol) in phosphorus oxychloride (108 g, 709 mmol) at 0°C. The mixturewas refluxed for 3 hours. The solvent was evaporated under vacuum. The residue wasdissolved in toluene (50 ml) and the solution was added to ice water (50 g). The organiclayer was separated and washed successively with water (2 x 50 ml), 10% aqueous NaHCO3 solution (2 x 50 ml), water (2 x 50 ml), brine (50 ml). The organic layer was dried (Mg504), filtered and the filtrate was concentrated under vacuum to yield intermediate 40 (1.91 g, 58.61%)1H NMR (400 MHz, CDC13) ? ppm 2.80 (s, 3 H) 3.00 (s, 3H) 7.41 (d, J=7.28 Hz, 1 H)7.68 - 7.76 (m, 1 H) 7.78 - 7.85 (m, 1 H).
References:
WO2016/91774,2016,A1 Location in patent:Page/Page column 48
56043-01-7
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147006-57-3
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4389-50-8
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