Thionation of phosphoramidodichloridates and phosphoramidate diesters using phosphorus pentasulfide and hexamethyldisiloxane under microwave irradiation. Part 1

Tetrahedron Letters

Volumn 45, Issue 37, 2004, Pages 6863-6866

  Nivsarkar, Manisha ^a   Gupta, Arvind K ^a   Kaushik, Mahabir P ^a  

^a Process Technology Development Division   (India)

Author keywords

HMDO; Microwave irradiation; Phosphoramidate diesters; Phosphoramidodichloridates; Phosphorus pentasulfide; Solvent free

Indexed keywords

ESTER DERIVATIVE; HEXAMETHYLDISILOXANE; PHOSPHORAMIDIC ACID DERIVATIVE; PHOSPHORUS DERIVATIVE;

ARTICLE; CHEMICAL ANALYSIS; CHEMICAL PROCEDURES; CHEMICAL REACTION; MICROWAVE IRRADIATION; REACTION ANALYSIS; SYNTHESIS;

EID: 4344655930     PISSN: 00404039     EISSN: None     Source Type: Journal    
DOI: 10.1016/j.tetlet.2004.07.099     Document Type: Article

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22. 10 (0.8 mmol), and HMDO (1.5 mmol) were taken in a 250 mL conical flask and mixed thoroughly on a cyclomixer. After initial exposure for 30 s in a MW oven at a power level of 900 W, the flask was taken out, shaken for 10 s and then exposed to the same MW power for further periods of time as indicated in Table 1 until the formation of the thio compounds was virtually complete. The recorded internal temperature of the reaction mixture was 110-C. The progress of the reaction was monitored by TLC (silica plates, 10% acetone in toluene) and GC. After the completion of reaction, the reaction mixture was dissolved in dichloromethane, filtered, concentrated, and purified by column chromatography (silica 60-120 mesh), using toluene as the eluent