Continuously updated synthesis method about 15666-97-4

According to the analysis of related databases, 15666-97-4, the application of this compound in the production field has become more and more popular.

Reference of 15666-97-4, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 15666-97-4 as follows.

Under argon gas protection, to a two-ported flask filled with 3T(OEH-BDT)3T(CHO)2 (360 mg, 0.2 mmol), octyl cyanoacetate (10-fold molar equivalent) and 100 mL of dry trichloromethane was added dropwise several drops of triethylamine. The mixture was stood at room temperature overnight. The mixture was poured into 100 mL of water and extracted with dichloromethane (30 mL¡Á3). The organic phase was washed with water (60 mL), saturated saline (60 mL) and water (60 mL), successively. The organic phase was dried over anhydrous sodium sulfate. After the solvent was removed under reduced pressure, the resultant product was separated with chromatographic column, in which petroleum ether-dichloromethane (1:2) was eluant, to give a brown solid (yield: 91%). MALDI-TOF MS (m/z): C106H148N2O4S8 [M]+, calculated: 1800.91; found: 1800.90.

According to the analysis of related databases, 15666-97-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; NANKAI UNIVERSITY; Chen, Yongsheng; Wan, Xiangjian; Liu, Yongsheng; Li, Zhi; Zhou, Jiaoyan; Wang, Fei; He, Guangrui; Long, Guankui; US9184315; (2015); B2;,
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