Synthesis of spiro-fused (C5)-isoxazolino-(C4)-pyrazolones (1-oxa-2,7,8-triazaspiro[4,4]-2,8-dien-6-ones) via 1,3-dipolar cycloaddition and cycloelimination

An efficient and selective method for the synthesis of spiro-fused (C5)-isoxazolino-(C4)-pyrazolones (C) is reported. The process consists of utilizing the Baylis-Hillman reaction-or a quicker, stepwise MAC procedure-to give I followed by 1,3-dipolar cycloaddition and Swern oxidation to give beta-ketoesters H, which were condensed with hydrazine derivatives to provide hydrazones that underwent cycloelimination. These novel spiro-fused (C5)-isoxazolino-(C4)-pyrazolones were confirmed by spectroscopic analysis as well as single-crystal X-ray of 5. We also concluded that all condensations/cycloeliminations, except with hydrazine itself, were more effective with catalysts or higher reaction temperatures. For example, TiCl(4) was an efficient catalyst for hydrazone formation and cycloelimination with methylhydrazine, while phenyl-, benzyl-, and (4-methoxyphenyl)hydrazine reacted effectively without catalyst in refluxing xylene.     

大气环境监测车载激光雷达系统通过鉴定

2005年7月14日，中科院综合计划局会同基础科学局对中国科学院安徽光学精密仪器研究所承担的奥运科技项目——“大气污染预报、预测和预警技术和设备研究——车载激光雷达”进行了验收。同时，该所研究的“AML-2车载式大气环境监测激光雷达系统”也一同通过了中科院组织的成果鉴定。