一二三四区视频,亚洲少妇熟女色,日本久热无码视频网,欧美国产日韩大尺度,亚洲a视频,久久少妇一区二区,日韩999无码视频,刺激久久久久久久,啊啊啊啊不要啊在线

Welcome to chemicalbook!
Chinese English Japanese Germany Korea
010-86108875
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List 6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI)
315228-79-6

6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI) synthesis

7synthesis methods
Potassium ethylxanthate

140-89-6

4-AMINO-2-IODOBENZONITRILE  98

33348-34-4

6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI)

315228-79-6

The general procedure for the synthesis of 2-mercaptobenzothiazole-6-carbonitrile from potassium ethylxanthate and 4-amino-3-iodobenzonitrile was as follows: 4-amino-3-iodobenzonitrile (0.6 mmol), potassium ethylxanthate (1.8 mmol), FeF3 (0.06 mmol), 2,2'-bis(diphenylphosphino)-1,1'-binaphthyl ( 0.03 mmol) and DMF (4 mL). The reaction vessel was replaced three times with argon and sealed. Subsequently, the mixture was placed in an oil bath at 110 °C and the reaction was electromagnetically stirred for 3-21 hours. The reaction process was monitored by silica gel thin layer chromatography (TLC). After completion of the reaction, the reaction mixture was cooled to room temperature, 4 mL of 3 mol/L hydrochloric acid solution was added and stirred for 30 min. The reaction mixture was extracted with ethyl acetate (3 x 20 mL). The organic phases were combined, dried with anhydrous sodium sulfate, and finally purified by silica gel column chromatography (eluent: petroleum ether/ethyl acetate) to obtain the target product 2-mercaptobenzothiazole-6-carbonitrile.

-

Yield:315228-79-6 98%

Reaction Conditions:

with iron(III) trifluoride;2,2'-bis-(diphenylphosphino)-1,1'-binaphthyl in N,N-dimethyl-formamide at 110; for 10 h;Inert atmosphere;Sealed tube;

Steps:

2. General experimental procedure

General procedure: A 25 mL reaction tube was charged with 2-haloaniline 1 (0.6 mmol), potassium o-ethyldithiocarbonate 2 (1.8 mmol), FeF3 (0.06 mmol), 2,2’-bis(diphenylphosphino)-1,1’-binaphthyl (0.03 mmol) and DMF (4 mL). The reaction vessel was flushed with argon for three times and sealed. Then the mixture was stirred electromagnetically in an oil bath at 110 for 3 - 21 hours. The reaction process was monitored by TLC on silica gel. After the reaction was completed, the reaction mixture was cooled to room temperature, then 4 mL HCl (3mol/L) was added and stirred for 30 minutes. Then the reaction mixture solution was extracted by ethyl acetate (3*20 mL). Subsequently, the combined organic solution were dried by anhydrous sodium sulfate and the target product was purified by silica gel colum chromatography (eluent: petroleum ether / ethylacetate) to give the corresponding pure product 3.

References:

Gao, Min;Lou, Chunqing;Zhu, Ning;Qin, Weijing;Suo, Quanling;Han, Limin;Hong, Hailong [Synthetic Communications,2015,vol. 45,# 20,p. 2378 - 2385] Location in patent:supporting information

6-Benzothiazolecarbonitrile,2,3-dihydro-2-thioxo-(9CI) Related Search:

达拉特旗| 祁连县| 德兴市| 舞阳县| 克山县| 武清区| 大石桥市| 泸定县| 大悟县| 西峡县| 泌阳县| 宾阳县| 翁源县| 巫山县| 长岭县| 清水河县| 政和县| 黄浦区| 山西省| 重庆市| 南丰县| 上栗县| 思茅市| 凤阳县| 常德市| 托克托县| 永修县| 福贡县| 白河县| 措美县| 陵川县| 庄河市| 古丈县| 通城县| 中牟县| 利辛县| 新化县| 乳山市| 平湖市| 神农架林区| 施甸县|