10-METHYLPHENOTHIAZINE synthesis
- Product Name:10-METHYLPHENOTHIAZINE
- CAS Number:1207-72-3
- Molecular formula:C13H11NS
- Molecular Weight:213.3
92-84-2
74-88-4
1207-72-3
General procedure for the synthesis of 10-methylphenothiazine from phenothiazine and iodomethane: NaH (60% purity, 1.0 g, 25.1 mmol) was slowly added to a 50 ml round-bottomed flask containing DMF (10 ml) under ice-water bath conditions. Iodomethane (1.3 g, 11.04 mmol) and phenothiazine (2 g, 10.0 mmol) were then added sequentially. The reaction mixture was transferred to room temperature and stirred for 2 h. The progress of the reaction was monitored by TLC. After completion of the reaction, the reaction was quenched by addition of water and extracted with dichloromethane (50 ml x 3). The organic phases were combined and dried with magnesium sulfate and subsequently concentrated to remove the solvent. Purification by silica gel column chromatography afforded the target product 10-methylphenothiazine (2.1 g, white solid) with a melting point of 96 °C in 97% yield.
Yield:1207-72-3 97%
Reaction Conditions:
with sodium hydride in N,N-dimethyl-formamide;mineral oil at 20; for 2 h;Cooling with ice;
Steps:
1
Weighing NaH (60% purity, 1.0g, 25 . 1mmol) is slowly added in the ice water bath in DMF (10 ml) of 50 ml round bottom bottle in, subsequently adding methyl iodide (1.3g, 11 . 04mmol) and compound phenothiazine (2g, 10.0mmol), transfer to room temperature stirring 2h, TLC monitoring after the reaction, water, for extracting DCM (50 ml x 3), magnesium sulfate drying and then concentrated dry, separate the product by silica gel column 1a (2.1g), white solid, melting point: 96 °C, yield 97%.
References:
Guangdong University of Technology;Chen, Huixiong;Pascal, Dao;Guo, Qihui;Ye, Feifei CN106045986, 2016, A Location in patent:Paragraph 0039; 0040; 0041
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