碘代咔唑类DNMT抑制剂中间体的合成

Synthesis of DNMT Inhibitor Intermediate with Iodine Substituted Carbazole

以咔唑和碘为原料,经碘化、N-烷基化、开环得到目标化合物1,3-双(3,6-二碘-9H-咔唑-9-基)-2-丙醇,总收率36.5%。产物的结构经~1HNMR、^(13)CNMR和MS表征。对基于I_2/DMSO体系的关键碘化反应进行了机理阐释和条件优化,确定了最优反应条件为n(咔唑)∶n(I_2)=2∶3,110℃下反应4 h,平均产率为85.2%。

1,3-Bis（3,6-diiodo-9H-carbazol-9-yl） propan-2-ol was synthesized from carbazole and iodine by iodination,N-alkylation and ring-opening. The total yield is 36. 5%. The target compounds were confirmed with-1HNMR,-（13）CNMR and MS. The mechanism of the key iodination based on the I_2/DMSO system was explained and the condition of iodination was optimized. In the presence of n（carbazole） ∶ n（I_2） = 2∶ 3 as starting materials,DMSO as solvent,4 h under 110 ℃,the average yield of the iodination was up to 85. 2%.