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Showing posts with label Diethyl Chlorophosphate. Show all posts
Showing posts with label Diethyl Chlorophosphate. Show all posts

Friday 22 September 2017

Diethyl Chlorophosphate


 
 
Diethyl Chlorophosphate (CAS no 814–49–3)(15)
Preparative Procedure
In a dry four-neck 250 mL round-bottom flask equipped with a mechanical stirrer, a thermometer, and an argon inlet were introduced at 20 °C triethylamine (21.3 g, 210 mmol), tert-butyl methyl ether (75 mL), and ethanol (9.67 g, 210 mmol). Phosphorus oxychloride (15.3 g, 100 mmol) was added dropwise in 10 min via a syringe; the temperature was maintained below −5 °C. Then, the cooling bath was removed and the white suspension was vigorously stirred during 5 h at 20 °C. The mixture was filtered and the solid was rinsed with 3 × 100 mL of diethyl ether. The solvents were removed under vacuo. The resulting crudez product was distilled under reduced pressure to afford 15.4 g (89% yield) of diethyl chlorophosphate containing 3% of triethylphosphate.
Eb3 = 51 °C (lit:(3) Eb10 = 85–87 °C).
 
1H NMR (CDCl3, 300 MHz, δ): 1.37 (6H, t, J = 6.0 Hz), 4.16–4.30 (4H, m).
 
13C NMR (CDCl3, 75 MHz, δ): 15.6 (d, J = 7.5 Hz), 65.7 (d, J = 6.8 Hz).
 
 
31P RMN (CDCl3, 121 MHz, δ): 4.5.
 
15AcharyaJ.GuptaA. K.ShakyaP. D.KaushikM. P. Tetrahedron Lett. 2005465293 DOI: 10.1016/j.tetlet.2005.06.024
 
str1 str2 str3
 
 

Eco-Friendly and Industrially Scalable Synthesis of the Sex Pheromone of Lobesia botrana. Important Progress for the Eco-Protection of Vineyard

 Chimie ParisTech, PSL Research University, CNRS, Institut de Recherche de Chimie Paris (IRCP), F-75005 Paris, France
 M2i, Route Nationale 117, Lotissement Induslacq, 64170 Lacq, France
§ Université Paris 13, 74 rue Marcel Cachin, 93017 Bobigny, France
Org. Process Res. Dev., Article ASAP
DOI: 10.1021/acs.oprd.7b00206
 
 
氯磷酸二乙酯
 
 
 
氯磷酸二乙酯
 
 
 
氯磷酸二乙酯
 
http://www.rsc.org/suppdata/c6/nj/c6nj03712g/c6nj03712g1.pdf