摘要
以双三氯甲基碳酸酯(三光气,简称BTC)代替三氯氧磷与D(-)-α-(4-乙基-2,3-双氧代哌嗪-1-甲酰胺基)对羟基苯乙酸(OH-EPCP)发生酰氯化反应制备4-乙基-2,3-双氧代哌嗪-1-甲酰胺基-对羟基苯乙酰氯(OH-EPCP氯化物)。当酰氯化条件为:n(OH—EPCP)／n(BTC)=3／1,三乙胺(TEA)为引发剂,反应温度为0～5℃,反应时间2．5 h时,目标产物收率达97.6％。产品为淡黄色粉末,用高效液相色谱仪测得w(OH—EPCP氯化物)=98．14％。用红外光谱仪分析产品主要官能团(cm-1):3431,1789,1716,1682,1614、1517、1472,1188,790～860,683。1H NMR(CDCl3)分析结果(δH):11．716,7．196,6．890,5．314,4．021,3．518-3．541,3．073,1．369。
4-ethyl-2,3-dioxopiperazine-l-carboxamido-p-hydroxyphenylacetyl chloride was prepared from D （-）-α-（4-Ethyl-2,3-dioxopiperazine-l-carboxamido）-p-hydroxyphenylacetic acid （OH-EPCP） by the reaction of bis（trichloromethyl） carbonate （triphosgene or BTC） instead of POC13. When the reaction conditions were as follows： the mole ratio n（OH-EPCP）/n（BTC）was 3/1 at the temperature of 0-5℃ for 2.5 h with triethylamine as catalyst, and the product of light yellow powder product was obtained in yield of 97.6 %. Weight percent of the product was 98.14 %, which was measured by HPLC. The main functional group were analyzed by IR. 3431,1789, 1716,1682,1614,1517,1472,1188,790-86 and 683,and the results of ^1-I NMR（CDCl3）were. 11. 716,7. 196,6.890,5.314,4. 021,3.518-- 3.541,3. 073 and 1. 369.
出处
《广州化工》
CAS
2006年第5期1-3,共3页
GuangZhou Chemical Industry
