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Multi-stage Reactions in One-pot using Inorganic Supported Reagents

使用无机支持试剂的一锅多级反应

基本信息

批准号：
11650875
负责人：
KODOMARI Mitsuo
金额：
$ 1.86万
依托单位：
Shibaura Institute of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
1999
资助国家：
日本
起止时间：
1999 至 2000
项目状态：
已结题

项目摘要

We have investigated two-stage reactions in one-pot using inorganic supported reagents on the assumption that two reagents reacting each other in homogenous solution are rendered mutually inactive by supporting them onto separate inorganic supports. It should be possible that two-step synthesis, in which a soluble reagent (A) react first with one supported reagent (Y) and the product (B) with the second supported reagent (X) to give the desired final product (C). Typically, 2-aminothiazoles are prepared either by the condensation of α-halo ketones with monosubstituted thioureas or by the reaction of α-thiocyanato carbonyl compounds with aromatic or aliphatic amine hydrochlorides. We have developed a convenient method for the preparation of 2-aminothiazoles in one-pot from readily available α-halo ketones using supported reagents system KSCN/SiO_2-RNH_3AcO/Al_2O_3. α-Halo ketones react first with KSCN/SiO_2 affording α-thiocyanates, the latter moving to RNH_3AcO/Al_2O_3 and reactins with it to give the end product 2-aminothiazoles. We have also developed one-pot synthesis of α-alkylthio-β-diketones from-β-diketones and thiols using supported reagents system CuBr_2/Al_2O_3-NaOH/Al_2O_3. β-Diketones react with CuBr_2/Al_2O_3 to give α-bromo-β-diketones, and then the bromides react with thiols in the presence of the base NaOH/Al_2O_3 to afford the end product α-alkylthio-β-diketones.

我们研究了使用无机载体试剂的一锅两步反应，假设在均相溶液中相互反应的两种试剂通过将它们支撑在单独的无机载体上而变得相互不活跃。两步合成应该是可能的，其中可溶试剂(A)首先与一种载体试剂(Y)反应，产物(B)与第二载体试剂(X)反应，得到所需的最终产品(C)。通常，通过α-卤代酮与单取代硫脲的缩合或通过α-硫氰酸酯化合物与芳香胺或脂肪胺盐酸盐的反应制备2-氨基噻唑。本文提出了一种简便的一锅法合成2-氨基噻唑类化合物的方法。该方法采用负载型试剂体系KSCN/SiO_2-RNH_3AcO/Al_2O_3。α-卤代酮首先与KSCN/SiO_2反应生成α-硫氰酸酯，然后转移到RNH_3AcO/Al_2O_3上，再与其反应生成2-氨基噻唑。我们还利用负载型试剂体系CuBr2/Al_2O_3-NaOH/Al_2O_3，以-α-二酮和硫醇为原料，一锅法合成了α-烷基-硫代-β-二酮。β-二酮与CuBr2/Al_2O_3反应生成α-溴-β-二酮，再与硫醇在碱性氢氧化钠/Al_2O_3存在下反应生成α-烷基硫代-β-二酮。