上海化工
上海化工
상해화공
SHANGHAI CHEMICAL INDUSTRY
2011年
10期
11-13
,共3页
程文峰%张雯君%徐晓东%杨巧梅
程文峰%張雯君%徐曉東%楊巧梅
정문봉%장문군%서효동%양교매
4-甲基邻苯二甲腈%4-甲基苯酐%酰胺脱水%三氯氧磷%合成
4-甲基鄰苯二甲腈%4-甲基苯酐%酰胺脫水%三氯氧燐%閤成
4-갑기린분이갑정%4-갑기분항%선알탈수%삼록양린%합성
Synthesis 4-methytphthalonitrile%4-methylphthalic anhydride%Amide dehydration%Phosphorus oxyeldoride
介绍了一种采用酰胺脱水法合成4-甲基邻苯二甲腈的方法，同时考察了反应温度、时间和脱水试剂等因素对收率的影响。以4-甲基苯酐为原料，通过氨解反应得到4-甲基邻苯二甲酰胺，再经过脱水反应得到扣甲基邻苯二甲腈。同时确定了脱水反应的最佳条件：选择三氯氧磷为脱水试剂，65-70℃反应5h。产物经红外结构鉴定，总收率为74。7％。结果表明：实验所提合成路线可行，且具有工艺简单、收率高、反应温和等特点.
介紹瞭一種採用酰胺脫水法閤成4-甲基鄰苯二甲腈的方法，同時攷察瞭反應溫度、時間和脫水試劑等因素對收率的影響。以4-甲基苯酐為原料，通過氨解反應得到4-甲基鄰苯二甲酰胺，再經過脫水反應得到釦甲基鄰苯二甲腈。同時確定瞭脫水反應的最佳條件：選擇三氯氧燐為脫水試劑，65-70℃反應5h。產物經紅外結構鑒定，總收率為74。7％。結果錶明：實驗所提閤成路線可行，且具有工藝簡單、收率高、反應溫和等特點.
개소료일충채용선알탈수법합성4-갑기린분이갑정적방법，동시고찰료반응온도、시간화탈수시제등인소대수솔적영향。이4-갑기분항위원료，통과안해반응득도4-갑기린분이갑선알，재경과탈수반응득도구갑기린분이갑정。동시학정료탈수반응적최가조건：선택삼록양린위탈수시제，65-70℃반응5h。산물경홍외결구감정，총수솔위74。7％。결과표명：실험소제합성로선가행，차구유공예간단、수솔고、반응온화등특점.
This paper introduced a synthetic method of 4-methyl phthalonitrile by amide dehydration and at the same time,the reaction temperature, time and dehydrating agent were examed and optimized as the factors of the yield, which can reached 74.7% in the optimum condition： 4-methyl phthalonitrile was synthesized from 4- methylphthalic anhydride to 4-methyl phthaldiamide by ammonolysis and dehydrated by phosphorus oxyehloride. The reaction temperature was 65-70 ℃ and reaction time was 5 hours. The product was identified by infrared structure. The results indicated that this synthesis route was feasible, characterized with simple process, high yield and in mild route.
