请求大神帮忙翻译一段英文文献不胜感激!!!!!!!太难了 ,有机化学类的 5

dl-2-Methyl-5-isopropyl-7-cyano-1,J-heptadiene(VII).-Triphenylphosphinewithexcess3-ch... dl-2-Methyl-5-isopropyl-7-cyano-1,J -heptadiene (VII) .-Triphenylphosphine
with excess 3-chloro-2-methylpropene in refluxing
dry benzene gave a 98% yield of methallyltriphenylphosphonium
chloride in 2 weeks. The product crystallized as it was
formed and was removed at intervals by filtration and utilized
without further purification.
A solution of n-butyllithium (215 ml., 1.62 N , 0.348 mole) in
hexane was slowly added to a stirring suspension of methallyltriphenylphosphonium
chloride (129 g., 0.366 mole) in 500 ml.
of tetrahydrofuran (freshly distilled from LiAlH4) under a nitrogen
atmosphere. The resulting intensely red solution of methallylidenetriphenylphosphorane
was stirred for 16 hr. at 20' and
then VI (30.6 g., 0.220 mole) in 35 ml. of dry tetrahydrofuran
was slowly added. The mixture was stirred at room temperature
for 1 hr . , refluxed for 3 hr . , and then concentrated under vacuum.
Water was added to the residue and the mixture was extracted
several times with hexane after which the combined hexane extracts
were cooled to 0" and filtered to remove triphenylphosphine
oxide. Fractional distillation of the hexane-soluble materials gave
VI1 (32.64 g., 83.9%), b.p. 67-73' (0.9 mm.). The higher boiling
fractions were almost entirely the 3,4-trans product while
some of the 3,4-&-cyanodiene was found in the lower boiling
fractions. A pure sample of 3,4-trans-VII was obtained by g.1.c.
(PDEAS) and had ~ Z O D1 .4795 and dZ040 .872.
展开
z1450613247
2013-03-16
知道答主
回答量:41
采纳率:0%
帮助的人:21.3万
展开全部
dl 2甲基5异丙7含氰基的1,J庚二烯(VII)三苯基膦
3-chloro-2-methylpropene过剩在回流
干苯98%的收益率methallyltriphenylphosphonium给的
氯在2周。产品结晶一样
形成和被删除间隔以过滤和利用
没有进一步的净化。
一个解决方案的n-butyllithium(215毫升,1.62 N,0.348摩尔)
己烷是缓慢加入到搅拌methallyltriphenylphosphonium暂停
氯(129 g。,0.366摩尔)在500毫升。
的四氢呋喃(新鲜蒸馏从LiAlH4)在氮气
气氛。由此产生的强烈的红色methallylidenetriphenylphosphorane溶液
了16人力资源。在20和
然后六世(30.6 g。,0.220摩尔)在35毫升干燥的四氢呋喃
慢慢地补充道。混合物在室温下都惊动了
为1小时。,refluxed 3人力资源。,然后集中在真空。
水被添加到残渣和混合物中提取
多次与己烷之后,结合己烷提取物
被冷却到0”和过滤去除三苯基膦
氧化物。分馏的己烷可溶性材料给了
VI1(32.64 g。,83.9%)、b p。67 - 73”(0.9毫米)。较高的沸点
分数几乎完全是3、4反式产品的同时
一些3、4 -&-cyanodiene被发现在低沸点
分数。一个纯样品3、4反式vii得到g 1 c。
(PDEAS)和有~ Z O D1。4795年和dZ040 .872。
绅士老总bc
2013-04-08 · TA获得超过5960个赞
知道大有可为答主
回答量:2809
采纳率:44%
帮助的人:1627万
展开全部
dl-2-methyl-5-isopropyl-7-cyano-1,J -庚二烯(七)-三苯基膦。
在回流的多余的3 -氯-2 -甲基丙烯
干了methallyltriphenylphosphonium苯收率98%
在2周的氯化物。该产品是结晶
形成和删除的时间间隔,通过过滤和利用
没有进一步的纯化。
正丁基锂溶液(215毫升,1.62 N,0.348摩尔)在
正己烷慢慢加入搅拌悬浮methallyltriphenylphosphonium
氯(129克,0.366摩尔)在500毫升。
四氢呋喃(新鲜蒸馏从LiAlH4)在氮
气氛。由此产生的methallylidenetriphenylphosphorane强烈的红色溶液
搅拌16小时。在20和
然后VI(30.6克,0.220摩尔)在35毫升干燥四氢呋喃
慢慢加入。混合物在室温下搅拌
1小时。回流3小时。,然后经真空浓缩。
水的加入和混合的残渣中提取
几次后用正己烷,己烷提取物的组合
被冷却到0”和过滤去除三苯基膦
氧化物。正己烷可溶材料的分馏给
vi1(32.64克,83.9%),BP二四”(0.9毫米。)。高沸点
部分几乎完全3,4-trans产品而
一些3,4 -和- cyanodiene在低沸点的发现
分数。通过1是3,4-trans-vii纯样品。C。
(pdeas)和有~ Z O D1 dz040。4795和872。
已赞过 已踩过<
你对这个回答的评价是?
评论 收起
推荐律师服务: 若未解决您的问题,请您详细描述您的问题,通过百度律临进行免费专业咨询

为你推荐:

下载百度知道APP,抢鲜体验
使用百度知道APP,立即抢鲜体验。你的手机镜头里或许有别人想知道的答案。
扫描二维码下载
×

类别

我们会通过消息、邮箱等方式尽快将举报结果通知您。

说明

0/200

提交
取消

辅 助

模 式