陕西科技大学学报(自然科学版)
陝西科技大學學報(自然科學版)
협서과기대학학보(자연과학판)
JOURNAL OF SHAANXI UNIVERSITY OF SCIENCE & TECHNOLOGY
2014年
4期
71-74
,共4页
李运涛%范娇娇%沈文%王凡%邓李慧
李運濤%範嬌嬌%瀋文%王凡%鄧李慧
리운도%범교교%침문%왕범%산리혜
脯氨酸%二肽%液相合成%结构表征
脯氨痠%二肽%液相閤成%結構錶徵
포안산%이태%액상합성%결구표정
proline%dipeptide%solution-phase synthesis%characterization
以脯氨酸为原料在液相中合成了脯氨酰脯氨酸二肽(Pro-Pro ).通过正交试验对实验条件进行优化,确定了肽键形成的最佳温度为30℃、时间为20 h、投料摩尔比为1∶1.2、催化剂为N-羟基苯并三氮唑(HOBT )、溶剂为二氯甲烷(DCM ),产率达78%.产物经红外光谱(IR)和核磁共振氢谱(1 H NMR)进行结构表征,通过熔点测定和热重(TG)测试考察产物热性能.结果表明:IR中产物的C= O和C -N伸缩振动吸收峰分别出现在1689 cm -1和1397 cm -1处,均向高波数移动,说明产物中吡咯环具有较大张力;T G检测表明脯氨酰脯氨酸二肽的最高使用温度为155℃.
以脯氨痠為原料在液相中閤成瞭脯氨酰脯氨痠二肽(Pro-Pro ).通過正交試驗對實驗條件進行優化,確定瞭肽鍵形成的最佳溫度為30℃、時間為20 h、投料摩爾比為1∶1.2、催化劑為N-羥基苯併三氮唑(HOBT )、溶劑為二氯甲烷(DCM ),產率達78%.產物經紅外光譜(IR)和覈磁共振氫譜(1 H NMR)進行結構錶徵,通過鎔點測定和熱重(TG)測試攷察產物熱性能.結果錶明:IR中產物的C= O和C -N伸縮振動吸收峰分彆齣現在1689 cm -1和1397 cm -1處,均嚮高波數移動,說明產物中吡咯環具有較大張力;T G檢測錶明脯氨酰脯氨痠二肽的最高使用溫度為155℃.
이포안산위원료재액상중합성료포안선포안산이태(Pro-Pro ).통과정교시험대실험조건진행우화,학정료태건형성적최가온도위30℃、시간위20 h、투료마이비위1∶1.2、최화제위N-간기분병삼담서(HOBT )、용제위이록갑완(DCM ),산솔체78%.산물경홍외광보(IR)화핵자공진경보(1 H NMR)진행결구표정,통과용점측정화열중(TG)측시고찰산물열성능.결과표명:IR중산물적C= O화C -N신축진동흡수봉분별출현재1689 cm -1화1397 cm -1처,균향고파수이동,설명산물중필각배구유교대장력;T G검측표명포안선포안산이태적최고사용온도위155℃.
Pro-Pro was synthesized in solution phase with proline as the starting material .The experimental condition was optimized by orthogonal test in this paper .The maximum yield 78% was obtained when reaction temperature was 30 ℃ ,time was 20 h ,mole ratio was 1∶1 .2 with HOBT as catalyzer and DCM as solvent .The structure of products was charac-terized by IR Spectrum and 1 H NMR ,the thermal properties was analyzed by melting point and TG .Results showed :Pro-Pro as tertiary amides ,C= O and C -N stretching vibration absorption peak move to high wave number 1 689 cm -1 and 1 397 cm -1 ,which indicated pyr-role rings in proline has larger tension and strengthen bond vibration .The maximum service temperature of Pro-Pro was 155 ℃ indicated by TG test .