厦门大学学报（自然科学版）
廈門大學學報（自然科學版）
하문대학학보（자연과학판）
JOURNAL OF XIAMEN UNIVERSITY (NATURAL SCIENCE)
2009年
4期
559-563
,共5页
陈国钦%黎四芳%叶国梁%许玉君
陳國欽%黎四芳%葉國樑%許玉君
진국흠%려사방%협국량%허옥군
3%3-二甲基丁醛%氯化%催化氢化%合成
3%3-二甲基丁醛%氯化%催化氫化%閤成
3%3-이갑기정철%록화%최화경화%합성
3,3-dimethylbutyraldehyde%chlorination%catalytic hydrogenation%synthesis
3,3-二甲基丁醛是合成新型强力甜味剂纽甜的重要中间体,其生产成本对纽甜的生产和应用影响重大.报道了一种简便和经济的3,3-二甲基丁醛合成工艺,以3,3-二甲基丁酸为原料,经氯化反应和常压催化氢化反应,合成了3,3-二甲基丁醛.研究了反应的工艺条件.3,3-二甲基丁酸的氯化反应以氯化亚砜为氯化剂,较为适宜的工艺条件为n(氯化亚砜):n(3,3-二甲基丁酸)=1.3:1,反应温度80℃、反应时间3 h,3,3-二甲基丁酰氯的收率为92%.3,3-二甲基丁酰氯的常压催化氢化反应在二甲苯溶剂中进行,以Pd/C为催化剂,较为适宜的工艺条件为m(二甲笨):m(3,3-二甲基丁酰氯)=6.5:1,催化剂用量w=15%(基于3,3-二甲基丁酰氯),氢气流量90 mL/min,搅拌转速500 r/min,反应温度120℃, 反应时间6 h, 3,3-二甲基丁醛的收率为73.4%.催化剂重复使用6次,3,3-二甲基丁醛收率仍达到71%,显示良好的稳定性.
3,3-二甲基丁醛是閤成新型彊力甜味劑紐甜的重要中間體,其生產成本對紐甜的生產和應用影響重大.報道瞭一種簡便和經濟的3,3-二甲基丁醛閤成工藝,以3,3-二甲基丁痠為原料,經氯化反應和常壓催化氫化反應,閤成瞭3,3-二甲基丁醛.研究瞭反應的工藝條件.3,3-二甲基丁痠的氯化反應以氯化亞砜為氯化劑,較為適宜的工藝條件為n(氯化亞砜):n(3,3-二甲基丁痠)=1.3:1,反應溫度80℃、反應時間3 h,3,3-二甲基丁酰氯的收率為92%.3,3-二甲基丁酰氯的常壓催化氫化反應在二甲苯溶劑中進行,以Pd/C為催化劑,較為適宜的工藝條件為m(二甲笨):m(3,3-二甲基丁酰氯)=6.5:1,催化劑用量w=15%(基于3,3-二甲基丁酰氯),氫氣流量90 mL/min,攪拌轉速500 r/min,反應溫度120℃, 反應時間6 h, 3,3-二甲基丁醛的收率為73.4%.催化劑重複使用6次,3,3-二甲基丁醛收率仍達到71%,顯示良好的穩定性.
3,3-이갑기정철시합성신형강력첨미제뉴첨적중요중간체,기생산성본대뉴첨적생산화응용영향중대.보도료일충간편화경제적3,3-이갑기정철합성공예,이3,3-이갑기정산위원료,경록화반응화상압최화경화반응,합성료3,3-이갑기정철.연구료반응적공예조건.3,3-이갑기정산적록화반응이록화아풍위록화제,교위괄의적공예조건위n(록화아풍):n(3,3-이갑기정산)=1.3:1,반응온도80℃、반응시간3 h,3,3-이갑기정선록적수솔위92%.3,3-이갑기정선록적상압최화경화반응재이갑분용제중진행,이Pd/C위최화제,교위괄의적공예조건위m(이갑분):m(3,3-이갑기정선록)=6.5:1,최화제용량w=15%(기우3,3-이갑기정선록),경기류량90 mL/min,교반전속500 r/min,반응온도120℃, 반응시간6 h, 3,3-이갑기정철적수솔위73.4%.최화제중복사용6차,3,3-이갑기정철수솔잉체도71%,현시량호적은정성.
3,3-Dimethylbutyraldehyde(DMBD) is an important intermediate which is useful in the preparation of the novel high-intensity sweetener neotame.The cost of DMBD has a great influence on the production and application of neotame,therefore,a cost reduction is highly desirable.A convenient and economical method for preparation of DMBD is developed.DMBD was synthesized from 3,3-dimethylbutanoic acid by chlorination and catalytic hydrogenation under atmospheric pressure.Appropriate operation conditions for the reactions were researched.A yield of 92% for 3,3-dimethylbutanoyl chloride was achieved by chlorination of 3,3-dimethylbutanoic acid with thionyl chloride under following conditions:molar ratio of thionyl chloride to 3,3-dimethylbutanoic acid being 1.3:1,reaction at 80℃ for 3 h.The catalytic hydrogenation of 3,3-dimethylbutanoyl chloride was carried out using xylene as a sovlent and Pd/C as catalyst.Yield of DMBD was reached up to 73.4% after reaction for 6 h under following conditions:mass ratio of xylene to 3,3-dimethybutanoyl chloride being 6.5:1,the catalyst dosage 15% (by mass of 3,3-dimethylbutanoyl chloride),stirring speed 500 r/min,hydrogen flow rate 90 mL/min and temperature 120℃.A yield of 71% for DMBD was still achieved with the catalyst recycled for six times,which indicated good stability for the catalyst.
