南京林业大学学报（自然科学版）
南京林業大學學報（自然科學版）
남경임업대학학보（자연과학판）
Journal of Nanjing Forestry University(Natural Science Edition)
2015年
5期
150-154
,共5页
曹明珍%徐徐%鲍名凯%王石发
曹明珍%徐徐%鮑名凱%王石髮
조명진%서서%포명개%왕석발
间二氯苯%甲醇钠%甲氧基化反应%间氯苯甲醚
間二氯苯%甲醇鈉%甲氧基化反應%間氯苯甲醚
간이록분%갑순납%갑양기화반응%간록분갑미
1%3?dichlorobenzene%sodium methoxide%methoxylation reaction%m?chloroanisole
以间二氯苯和甲醇钠为原料,对间氯苯甲醚合成的新工艺进行了研究;通过单因素实验考察了溶剂种类及用量、间二氯苯与甲醇钠的摩尔比、反应温度、反应时间对间二氯苯转化率和间氯苯甲醚得率的影响,并采用正交实验法对反应条件进行了优化. 确定了适宜的合成工艺条件为:以N,N-二甲基甲酰胺( DMF)作溶剂,溶剂用量为75 mL/mol,n(间二氯苯):n(甲醇钠)=1:1.2,反应温度为120 ℃,反应时间6 h. 在此工艺条件下,间二氯苯的转化率为94.8%,间氯苯甲醚的得率为91. 0%. 采用FT-IR和GC-MS分析技术对间氯苯甲醚进行了表征.
以間二氯苯和甲醇鈉為原料,對間氯苯甲醚閤成的新工藝進行瞭研究;通過單因素實驗攷察瞭溶劑種類及用量、間二氯苯與甲醇鈉的摩爾比、反應溫度、反應時間對間二氯苯轉化率和間氯苯甲醚得率的影響,併採用正交實驗法對反應條件進行瞭優化. 確定瞭適宜的閤成工藝條件為:以N,N-二甲基甲酰胺( DMF)作溶劑,溶劑用量為75 mL/mol,n(間二氯苯):n(甲醇鈉)=1:1.2,反應溫度為120 ℃,反應時間6 h. 在此工藝條件下,間二氯苯的轉化率為94.8%,間氯苯甲醚的得率為91. 0%. 採用FT-IR和GC-MS分析技術對間氯苯甲醚進行瞭錶徵.
이간이록분화갑순납위원료,대간록분갑미합성적신공예진행료연구;통과단인소실험고찰료용제충류급용량、간이록분여갑순납적마이비、반응온도、반응시간대간이록분전화솔화간록분갑미득솔적영향,병채용정교실험법대반응조건진행료우화. 학정료괄의적합성공예조건위:이N,N-이갑기갑선알( DMF)작용제,용제용량위75 mL/mol,n(간이록분):n(갑순납)=1:1.2,반응온도위120 ℃,반응시간6 h. 재차공예조건하,간이록분적전화솔위94.8%,간록분갑미적득솔위91. 0%. 채용FT-IR화GC-MS분석기술대간록분갑미진행료표정.
A new preparation process for m?chloroanisole was explored from 1,3?dichlorobenzene and sodium methoxide. The effects of types of solvent and their dosage, mole ratio of 1,3?dichlorobenzene to sodium methoxide, reaction temper?ature and reaction time on the conversion rate of 1,3?dichlorobenzene and yield of m?chloroanisole was examined. The optimum synthesis conditions were obtained by orthogonal test as follows:N, N?dimethyl?formamide ( DMF) was used as solvent, and solvent dosage was 75 mL/mol; the molar ratio of 1,3?dichlorobenzene to sodium methoxide was 1:1.2;reaction temperature was 120℃ and reaction time was 6 h. Under this optimum conditions, the conversion rate of 1,3-dichlorobenzene was 94.8% and the yield of 1,3?chloroanisole was 91.0%. The structure of the m?chloroanisole was ana?lyzed by FT?IR and GC?MS.
