Acetic acid, 2-(tributylphosphoranylidene)-, methyl ester synthesis
- Product Name:Acetic acid, 2-(tributylphosphoranylidene)-, methyl ester
- CAS Number:108269-37-0
- Molecular formula:C15H31O2P
- Molecular Weight:274.38
Yield:108269-37-0 97%
Reaction Conditions:
in dichloromethane;toluene;
Steps:
I Step I:
Step I:
methyl 2-(tributylphosphoranylidene)acetate
To a cold (0° C.) solution of tributylphosphane (5.00 mL, 20.0 mmol) in toluene (20 mL) under N2 atmosphere is added methyl 2-bromoacetate (1.90 mL, 20.1 mmol).
The resulting slurry is warmed to RT and stirred overnight under N2 atmosphere.
The resulting mixture is concentrated in vacuo, redissolved in CH2Cl2 (50 mL), washed sequentially with aqueous 1N NaOH (2*20 mL), H2O (20 mL), dried over MgSO4, filtered and concentrated to provide the title compound (5.35 g, 97% yield) as a colorless oil
References:
US2014/274930,2014,A1 Location in patent:Page/Page column
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