2-Amino-5-methylbenzoic acid(1) was acylated with acyl chlorides,then heated(together) with(acetic) anhydride to give 2-phenyl or 2-benzyl-6-methylbenzoxazin-4-one(3a3b),while compound 1 was (reacted) with p...2-Amino-5-methylbenzoic acid(1) was acylated with acyl chlorides,then heated(together) with(acetic) anhydride to give 2-phenyl or 2-benzyl-6-methylbenzoxazin-4-one(3a3b),while compound 1 was (reacted) with propanoic anhydride or trifluoroacetic anhydride to give 2-ethyl or 2-trifluoromethyl-6-methylbenzoxazin-4-one(3c3d) directly. Then,2-substituted 6-methylbenzoxazin-4-ones(3a3d) were heated together with formamide to afford 2-substituted 6-methyl-4(3H)-quinazolinones(4a4d),which were(converted) into the title compounds(5a5d) via brominating with N-bromosuccinimide in the presence of (PhCOO)2.The structures of all the intermediates and final products were confirmed with ESI-MS,1H NMR and elemental analysis.展开更多
1-(4-Acetylaminophenyl)-α-bromo-1-propanone was synthesized from 1-(4-acetylaminophenyl) propanone through α-hydrogen brominating using Br2 in ethanol as bromination agent,and the yield was 70.4%.The melting poi...1-(4-Acetylaminophenyl)-α-bromo-1-propanone was synthesized from 1-(4-acetylaminophenyl) propanone through α-hydrogen brominating using Br2 in ethanol as bromination agent,and the yield was 70.4%.The melting point of the target compound was tested and the structure was confirrmed by FT-IR and MS.The route with little pollution and less loss of solvent is practically valuable.展开更多
From α acetylthioformanilide and thio semicarbazide eight heterocyclic compounds of substituted phenylamino 6 metyl 1,2,4 triazine 3 thiones were synthesized.Their structures were confirmed by elemental analysis, 1HN...From α acetylthioformanilide and thio semicarbazide eight heterocyclic compounds of substituted phenylamino 6 metyl 1,2,4 triazine 3 thiones were synthesized.Their structures were confirmed by elemental analysis, 1HNMR,IR and MS.展开更多
Solubilities of 4-hydroxybenzaldehyde, 3-bromo-4-hydroxybenzaldehyde, 3,5 -dibromo-4-hydroxybenzaldehyde in chloroform were measured at temperatures ranging from 283.15 K to 323.15 K.The measurements of temperature an...Solubilities of 4-hydroxybenzaldehyde, 3-bromo-4-hydroxybenzaldehyde, 3,5 -dibromo-4-hydroxybenzaldehyde in chloroform were measured at temperatures ranging from 283.15 K to 323.15 K.The measurements of temperature and enthalpy of fusion of pure solutes were used for caculation of solubility by ideal solution model,which was higher than the experimental values.The very low solubility in chloroform was due to self association of solute molecules.A λh formula was used to fit the data and had shown good correlation results.展开更多
文摘2-Amino-5-methylbenzoic acid(1) was acylated with acyl chlorides,then heated(together) with(acetic) anhydride to give 2-phenyl or 2-benzyl-6-methylbenzoxazin-4-one(3a3b),while compound 1 was (reacted) with propanoic anhydride or trifluoroacetic anhydride to give 2-ethyl or 2-trifluoromethyl-6-methylbenzoxazin-4-one(3c3d) directly. Then,2-substituted 6-methylbenzoxazin-4-ones(3a3d) were heated together with formamide to afford 2-substituted 6-methyl-4(3H)-quinazolinones(4a4d),which were(converted) into the title compounds(5a5d) via brominating with N-bromosuccinimide in the presence of (PhCOO)2.The structures of all the intermediates and final products were confirmed with ESI-MS,1H NMR and elemental analysis.
文摘1-(4-Acetylaminophenyl)-α-bromo-1-propanone was synthesized from 1-(4-acetylaminophenyl) propanone through α-hydrogen brominating using Br2 in ethanol as bromination agent,and the yield was 70.4%.The melting point of the target compound was tested and the structure was confirrmed by FT-IR and MS.The route with little pollution and less loss of solvent is practically valuable.
文摘From α acetylthioformanilide and thio semicarbazide eight heterocyclic compounds of substituted phenylamino 6 metyl 1,2,4 triazine 3 thiones were synthesized.Their structures were confirmed by elemental analysis, 1HNMR,IR and MS.
文摘Solubilities of 4-hydroxybenzaldehyde, 3-bromo-4-hydroxybenzaldehyde, 3,5 -dibromo-4-hydroxybenzaldehyde in chloroform were measured at temperatures ranging from 283.15 K to 323.15 K.The measurements of temperature and enthalpy of fusion of pure solutes were used for caculation of solubility by ideal solution model,which was higher than the experimental values.The very low solubility in chloroform was due to self association of solute molecules.A λh formula was used to fit the data and had shown good correlation results.