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Pathfinder Cookbook - reaction details
Reaction id: 0210091039_04, verified by Personal Chemistry ©

1506

1440

product 4

Yield: N/A  Time: 1200s   Temperature: 200 °C

Chemicals
 Name MW [g/mol] Density [g/ml] Amount [mmol] Mass/Volume
533686 195.061 1.321 3.048 450.000 µl
122521 166.157 0.969 12.189 2090.000 µl
Product 1 252.247 1.000 0.000 0.000 µl

Keywords
Arbuzov reaction, Substitution

Comments
Synthesis: Temperature and reaction time used in this reaction is a suitable method for slow reactive primary bromides and iodides. It can also be used on reactive secondary bromides.

Purification: Excess of triethylphosphite and ethyl diethylphosphonate are removed after reaction using vacuum distillation (triethylphosphite 50°C-55°C and ethyl diethylphosphonate 70°C-75°C at 10-15 mbar). For this substrate no further purification was made. Crude NMR confirmed the structure of the product. It is recommended to purify the product on a silica column.

Instrument Settings
Absorption level: Normal
Pre-stirring time: 0s

References
Bhattacharya, A. K.; Thyagarajan, G. Chem. Rev. 1981, 81, 415 Arbuzov, B. A. Pure Appl. Chem. 1964, 9, 307

Analysis
 Method Purity Files
 crude GCMS 26  0210091039_04G.pdf