Electric Literature of 24332-20-5, These common heterocyclic compound, 24332-20-5, name is 1,1,2-Trimethoxyethane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
EXAMPLE 2 Concentrated hydrochloric acid (0.84 ml) was added to a stirred mixture of 2-methoxyacetaldehyde dimethyl acetal (12.6 g) and water (59 ml) and the resultant solution was heated to 40 C. for 2 hours. The solution was cooled to ambient temperature and basified to pH8 by the addition of a saturated aqueous sodium bicarbonate solution. The mixture so obtained was added to a stirred suspension of 6-amino-4-(3′,4′-difluoroanilino)quinazoline hydrochloride (6.4 g) in a mixture of glacial acetic acid (1.26 g) and ethanol (750 ml). Sodium cyanoborohydride (2.64 g) was added and the mixture was stirred at ambient temperature for 16 hours. The mixture was evaporated and the residue was partitioned between methylene chloride and water. The organic phase was dried (MgSO4) and evaporated. The residue was purified by column chromatography using increasingly polar mixtures of methylene chloride and methanol as eluent. There was thus obtained 4-(3′,4′-difluoroanilino)-6-(2-methoxyethylamino)quinazoline (5.2 g, 69%), m.p. 150-153 C.; NMR Spectrum: (CD3 SOCD3 +CD3 CO2 D) 3.33 (s, 3H), 3.43 (t, 2H), 3.63 (t, 2H), 7.5 (m, 5H), 7.96 (m, 1H), 8.56 (s, 1H); Elemental Analysis: Found C, 61.1; H, 4.9; N, 16.5; C17 H16 F2 N4 O 0.2H2 O requires C, 61.1; H, 4.95; N, 16.8%.
The synthetic route of 24332-20-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Zeneca Limited; US5942514; (1999); A;,
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