问题：大家帮我看看，这个是什么期刊？
类型：求助 (悬赏分:3分)
提问：quan
等级：▲▲
版块：文献检索技术、各类代理(wguoyong,wangjinyon,)
信誉：82%
回复：11
阅读：2533
时间：2005-07-07 19:56:15 编辑加入/取消收藏订制/取消短消息举报该贴

Org. Synth,1945,25,19
我到www.orgsyn.org去找，没有找到这篇文章。这个期刊，是哪个出版社出版的？
谢谢！

回复人：wguoyong,▲▲▲▲ (原来做药物化学的，现在从事表面活性剂/洗涤剂研究开发) 时间：2005-07-07 22:14:25 编辑

1楼

L: 2-Methylpyrrolidine, 9CI
24152912,216

Chapman Hall Number: HBN83-R
CAS Registry Number: 765-38-8

Molecular Formula: C5H11N
Molecular Weight: 85.149
Accurate Mass: 85.089149
Percentage Composition: C 70.53%; H 13.02%; N 16.45%ffler, K., Ber., 1910, 43, 2044, (synth, N-Me)
Wolff, P., Ber., 1925, 58, 404, (N-Ph)
Yur'ev, P. et al., J. Gen. Chem. USSR (Engl. Transl.), 1941, 11, 1128, (N-Ph)
Org. Synth., 1945, 25, 19, (synth, N-Me)
Elderfield, R.C. et al., J.A.C.S., 1950, 72, 1334, (N-isopropyl)
Karrer, P. et al., Helv. Chim. Acta, 1951, 34, 2202, (abs config)
Corey, E.J. et al., J.A.C.S., 1960, 82, 1657, (abs config, N-Me)
Ferles, M. et al., Coll. Czech. Chem. Comm., 1971, 35, 2057, (N-Ph)
Blomqvist, L. et al., Acta Chem. Scand., 1972, 26, 3203, (ord, N-Me)
Perie, J.J., Tetrahedron, 1972, 28, 675, (synth, N-Me)
Kostyanovsky, R.G. et al., Tetrahedron, 1974, 30, 39, (synth)
Ringdahl, B., Acta Chem. Scand., 1990, 44, 42, (N-nitroso)
Shustov, G.V. et al., J.C.S. Perkin 2, 1996, 1907-1914, (N-nitro)

[00038556-7] A20

回复人：wguoyong,▲▲▲▲ (原来做药物化学的，现在从事表面活性剂/洗涤剂研究开发) 时间：2005-07-07 22:15:36 编辑	2楼
你要的765-38-8文献，消息没发过去，发这儿吧！！

回复人：quan,▲▲ (学化学，要从娃娃抓起...) 时间：2005-07-07 23:26:27 编辑	3楼
谢谢。这好像不是贝尔斯坦的结果吧。期待贝尔斯坦的结果

回复人：quan,▲▲ (学化学，要从娃娃抓起...) 时间：2005-07-07 23:31:20 编辑	4楼
另外，不知道有没有电子版的Ber.

回复人：阿朗,▲ () 时间：2005-07-08 00:02:14 编辑	5楼
自己顶起走哦

回复人：wguoyong,▲▲▲▲ (原来做药物化学的，现在从事表面活性剂/洗涤剂研究开发) 时间：2005-07-10 22:00:25 编辑	6楼
http://free.ys168.com/?wguoyong to quan 有765-38-8的scifinder检索结果

回复人：qyl1970,★ (专注于有机合成，接受公斤级化合物定制。) 时间：2005-07-11 08:50:21 编辑	7楼
这是CCD的检索结果吧！不知有没有CCD可以共享?

回复人：netpanda,▲▲▲ (CHEM-IS-TRY!永远的求知者) 时间：2005-07-11 10:25:12 编辑	8楼
我想你的没有仔细的找,就是这个文章啊:Organic Syntheses, Vol. 25, p.19 = Coll. Vol. 3, p.169.也就是说是累积卷的第3卷第169页.自己去下吧.

回复人：netpanda,▲▲▲ (CHEM-IS-TRY!永远的求知者) 时间：2005-07-11 10:27:34 编辑

9楼

干脆我给你贴出来,看看是不是你要的那东西,然后决定去不去下载pdf格式的内容.
Organic Syntheses, Coll. Vol. 3, p.169; Vol. 25, p.19
β-CARBOMETHOXYPROPIONYL CHLORIDE
[Propionic acid, β-(chloroformyl)-, methyl ester]

Submitted by James Cason
Checked by C. F. H. Allen and C. V. Wilson.
1. Procedure
A. Methyl hydrogen succinate. A mixture of 400 g. (4 moles) of succinic anhydride (Note 1) and 194 ml. (4.8 moles) of methanol (Note 2) in a 1-l. round-bottomed flask is refluxed on a steam bath. After about 35 minutes the mixture is swirled frequently until it becomes homogeneous (this requires 15–30 minutes); the flask is then half immersed in the steam bath for an additional 30–25 minutes (Note 3).
The excess methanol is removed by distillation under reduced pressure (water pump) from a steam bath, and the residual liquid is poured into an 18- to 25-cm. evaporating dish which is cooled in a shallow pan of cold water. As the half ester crystallizes, it is stirred and scraped off the dish in order to prevent formation of a solid cake. After being dried to constant weight in a vacuum desiccator (5–8 days), the product weighs 502–507 g. (95–96%) and melts at 57–58° (Note 4) and (Note 5).
B. β-Carbomethoxypropionyl chloride. In a 1-l. flask (Note 6) bearing a reflux condenser are placed 264 g. (2 moles) of methyl hydrogen succinate and 290 ml. (4 moles) of thionyl chloride (Note 7), and the solution is warmed in a bath at 30–40° for 3 hours (Note 8). The condenser is replaced by a modified Claisen still head, the excess thionyl chloride is removed on a steam bath under reduced pressure, and the β-carbomethoxypropionyl chloride is distilled (Note 9) and (Note 10). The yield of colorless product is 270–278 g. (90–93%), b.p. 92–93°/18 mm. (Note 11) and (Note 12).
2. Notes
1. Eastman's succinic anhydride (m.p. 115–116°) was used.
2. Synthetic methanol was used. Since this anhydrous alcohol is hygroscopic, partly filled bottles that have been opened intermittently in the laboratory should be rejected.
3. Thirty minutes is allowed if solution resulted after 15 minutes of swirling; 25 minutes if 30 minutes was needed for homogeneity.
The time factor is very important. In one run in which the mixture was heated for a total of 55 minutes, a product was obtained which was shown by titration to contain about 6% of anhydride. Longer heating than that specified increases the yield of diester. Any change in quantity of materials used may necessitate a new set of conditions in order to obtain the maximum yield.
4. The checkers prefer the following procedure, which can be carried through in one day. A suspension of approximately one-half of the crude product in 750 ml. of carbon disulfide is warmed on a steam bath; two layers form, in which some solid remains in suspension. This is dissolved by the addition of 350 ml. of ether. The whole is chilled to 0°, and the solid is filtered by suction. The other half of the crude product is now dissolved in this filtrate, the solution is again chilled to 0°, and the solid is filtered. The combined yield of acid ester, m.p. 57–58°, is 438–449 g. (83–85%). A further 32–37 g. (6–7%) of less pure material (m.p. 56–57°) can be obtained by concentrating the filtrate to half its volume and chilling to 0°.
5. The product, which is sufficiently pure for the next step, contains at least 98% methyl hydrogen succinate as shown by titration or distillation through an 18-in. Podbielniak-type column.
6. Equipment with ground-glass joints is used throughout.
7. Eastman's thionyl chloride (b.p. 75–76°) was used. The checkers obtained equivalent yields of the chloride by using only 20% excess of thionyl chloride. The mixture was heated for 1 hour at 40°, allowed to stand overnight, and heated again for 2 hours at 40°.
8. Since hydrogen chloride is evolved, it is advisable to work in a hood or employ a gas trap.
9. An electric heating mantle is convenient.
10. Other boiling points are 85.5–87°/13 mm. and 89–90°/15 mm. The use of as low a pressure as possible is advisable, since the substance tends to lose methyl chloride and form succinic anhydride.
11. The submitter obtained the same yield when phosphorus pentachloride was used instead of thionyl chloride. Consistent results were obtained with the former reagent only when the acid chloride was distilled at pressures below 3 mm. (b.p. 58–59°/2.5 mm.).
12. Methyl hydrogen glutarate, ethyl hydrogen adipate, and ethyl hydrogen sebacate may be converted to the corresponding ester acid chlorides by this procedure in about the same yields. Distillation should be carried out rapidly at a pressure of 4 mm. or lower.
3. Discussion
Methyl hydrogen succinate has been prepared by heating succinic acid with methyl succinate,1 by treating ethyl succinate with sodium methoxide,2 and by heating succinic anhydride with methanol.3,4,5,6
β-Carbomethoxypropionyl chloride has been prepared from methyl hydrogen succinate by the use of thionyl chloride4,6 or phosphorus pentachloride.5

回复人：quan,▲▲ (学化学，要从娃娃抓起...) 时间：2005-08-07 18:11:10 编辑	10楼
接受答案了。

回复人：hnxiao,▲ (诚实做人) 时间：2005-08-08 19:47:16 编辑	11楼
接受答案了。

得分人：netpanda-2,

问题讨论没有结束...

您尚未进入本论坛,登录之后才可以回贴

9msec