Quetiapine IMpurity 1 synthesis
- Product Name:Quetiapine IMpurity 1
- CAS Number:3985-12-4
- Molecular formula:C12H11NS
- Molecular Weight:201.29
Yield:3985-12-4 82%
Reaction Conditions:
with copper dichloride;N,N`-dimethylethylenediamine at 110; for 24 h;Inert atmosphere;Green chemistry;
Steps:
General procedure for the synthesis of diphenylsulfanes by iodobenzenes and benzenethiols (2c-29c).
General procedure: An oven-dried Schlenk tube equipped with a Teflon valve was charged with a magnetic stir bar, CuCl2 (15 mol%), iodobenzenes a (0.3 mmol) and benzenethiols d (0.3 mmol). The tube was placed under vacuum for 20 min and backfilled with N2. Then DMEDA (0.35 mL) was added through a syringe. The reaction mixture was stirred at 110 °C for 24 h. The reaction was monitored by TLC. When iodobenzenes a was consumed completely, the reaction was stopped and cooled to room temperature, the crude reaction mixture was filtered through the filter paper with EtOAc (20 mL) for 3 times. The combined organic phase was washed with water (30mL × 3), then concentrated and the residue was purified directly by column chromatography on silica gel using petrol/EtOAc as eluent to give the pure products c.
References:
Shen, Guodong;Lu, Qichao;Wang, Zeyou;Sun, Weiwei;Zhang, Yalin;Huang, Xianqiang;Sun, Manman;Wang, Zhiming [Synthesis,2022,vol. 54,# 1,p. 184 - 198] Location in patent:supporting information
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