四硫化二磷(P 4 S 10)中的吡啶已长期用作硫代剂。现在已经以结晶形式分离出对水分敏感的试剂,并且已经通过X射线晶体学确定了详细的结构。已经研究了这种可储存试剂的去硫能力,并将其转移到诸如乙腈之类的溶剂中,在该溶剂中已证明其在合成上是有用的并且具有非凡的选择性。它的性能已经与所谓的Lawesson试剂(LR)进行了比较。特别有趣的是在相对较高的温度(约165°C)下以二甲基砜为溶剂进行硫磺化的结果。在这些条件下,例如,a啶酮和3-乙酰吲哚可以迅速转化为相应的亚硫代衍生物。甘氨酰甘氨酸类似地得到哌嗪去甲酮。在这些温度下 LR由于快速分解而效率低下。硫代产物通常更清洁并且更容易获得,因为在结晶试剂中,常规试剂P中始终存在杂质吡啶或LR中的4 S 10已被除去。
四硫化二磷(P 4 S 10)中的吡啶已长期用作硫代剂。现在已经以结晶形式分离出对水分敏感的试剂,并且已经通过X射线晶体学确定了详细的结构。已经研究了这种可储存试剂的去硫能力,并将其转移到诸如乙腈之类的溶剂中,在该溶剂中已证明其在合成上是有用的并且具有非凡的选择性。它的性能已经与所谓的Lawesson试剂(LR)进行了比较。特别有趣的是在相对较高的温度(约165°C)下以二甲基砜为溶剂进行硫磺化的结果。在这些条件下,例如,a啶酮和3-乙酰吲哚可以迅速转化为相应的亚硫代衍生物。甘氨酰甘氨酸类似地得到哌嗪去甲酮。在这些温度下 LR由于快速分解而效率低下。硫代产物通常更清洁并且更容易获得,因为在结晶试剂中,常规试剂P中始终存在杂质吡啶或LR中的4 S 10已被除去。
[EN] A THIONATION PROCESS AND A THIONATING AGENT<br/>[FR] PROCÉDÉ DE THIONATION ET AGENT DE THIONATION
申请人:VIRONOVA AB
公开号:WO2012104415A1
公开(公告)日:2012-08-09
A process for transforming a group >C=O (I) in a compound into a group >C=S (II) or into a tautomeric form of group (II) in a reaction giving a thionated reaction product, by use of crystalline P2S5·2 C5H5N as a thionating agent. A thionating agent which is crystalline P2S5·2 C5H5N
Continuous‐Flow Electrosynthesis of Benzofused S‐Heterocycles by Dehydrogenative C−S Cross‐Coupling
作者:Chong Huang、Xiang‐Yang Qian、Hai‐Chao Xu
DOI:10.1002/anie.201901610
日期:2019.5.13
Reported herein is the synthesis of benzofused six‐membered S‐heterocycles by intramolecular dehydrogenative C−S coupling using a modularflow electrolysis cell. The continuous‐flow electrosynthesis not only ensures efficient product formation, but also obviates the need for transition‐metal catalysts, oxidizing reagents, and supporting electrolytes. Reaction scale‐up is conveniently achieved through
The present invention provides a compound of Formula I:
wherein
R is hydrogen or methyl; and
Z is:
or a pharmaceutically acceptable salt thereof, and the use of compounds of Formula I for treating neurodegenerative diseases, such as Alzheimer's disease.
Facile synthesis of novel 6-methyl-5-phenyl-2-sulfido-1,2,3,5-tetrahydro-4<i>H</i>[1,2] oxazolo[4′,5′:5,6]pyrano[2,3-<i>d</i>][1,3,2]diazaphosphinines
作者:Tarik E. Ali、Mohamed A. Assiri、Somaia M. Abdel-Kariem、Ibrahim S. Yahia
DOI:10.1080/17415993.2018.1455837
日期:2018.9.3
ABSTRACT A number of 6-methyl-5-phenyl-2-sulfido-1,2,3,5-tetrahydro-4H[1,2]oxazolo[4′,5′: 5,6]pyrano[2,3-d][1,3,2]diazaphosphinines 4–11 were synthesized via an interaction of tetraphosphorus decasulfide and Lawesson’s reagent under different conditions with 6-amino-3-methyl-4-phenyl-4H-pyrano[3,2-d][1,2]oxazole-5-carbonitrile (3). The reaction mechanisms for these products were discussed. Structures