diisobutyl hydrogen phosphate synthesis
- Product Name:diisobutyl hydrogen phosphate
- CAS Number:6303-30-6
- Molecular formula:C8H19O4P
- Molecular Weight:210.21
17158-87-1
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Yield:6303-30-6 75%
Reaction Conditions:
with sodium hydroxide in tetrahydrofuran;water at 0;
Steps:
General procedure 2: synthesis of dialkyl hydrogen phosphates
General procedure: The corresponding alky chlorophosphate (1 equiv.) was dissolved in THF and the resulting colorless solution was cooled to 0 °C. Then, aqueous NaOH (1 M, 1 equiv.) was added dropwise. The resulting mixture was stirred vigorously at 0 °C for 30 min, then concentrated under reduced pressure. The residual wet white solid was extracted with Et2O and the organic layer was dried over MgSO4. After filtration, the resulting solution was concentrated under reduced pressure to yield the crude product as a viscous oil. The latter was dissolved in a saturated solution of NaHCO3 that was subsequently washed three times with the same amount of CH2Cl2. The aqueous layer was then acidified with HCl (1 M) until the pH value was between 0 and 1 and extracted with CH2Cl2 (3× 50 mL). The combined organic layers were dried over MgSO4, then concentrated under reduced pressure to yield pure dialkyl hydrogen phosphates. All products were stored at -17 °C under an atmosphere of argon. All characterization data can be found in the electronic supplementary information.
References:
Santschi, Nico;Geissbühler, Patrik;Togni, Antonio [Journal of Fluorine Chemistry,2012,vol. 135,p. 83 - 86] Location in patent:experimental part
78-83-1
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1189-24-8
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6303-30-6
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126-71-6
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6303-30-6
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