| 摘要 |
PURPOSE: A preparation method of 1,3,5-substituted 2,4,6-triiodobenzene derivatives by reacting 1,3,5-substituted benzene derivatives with iodine chloride(ICI) and a base is provided which gives a high-purity product in a high yield. CONSTITUTION: 2,4,6-Triiodobenzene derivatives(1) substituted in the 1,3,5-position are prepared by reacting 1,3,5-substituted benzene derivatives(2) with iodine chloride(ICI) and a base in a mixture solvent of methanol and dichloromethane(CH2Cl2) at 0-80°C for 0.5-60 hr. In formula, R1 is a hydroxy, amino or nitro group; R2, R3 are independently 1-5C alkyl, CO2R4 or COR5; R4 is H or C1-7 alkyl; R5 is 1-3C alkyl amino, -N(R6)CH2CH(OR7)CH2OR7, -N(R6)CH(CH2OR7)CH(OR7)CH(OR7)CH2OR7 or -N(R6)CH(CH2OR7)CHOR7(R6,R7 are independently H, 1-2C alkyl or 1-3C acyl). The mixture ratio of methanol to dichloromethane is 1: 1 - 10: 1. The product is useful as an important intermediate of a contrast medium of X-rays.
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