4-Methyl-1,4-azaphosphinane 4-oxide synthesis
- Product Name:4-Methyl-1,4-azaphosphinane 4-oxide
- CAS Number:945460-43-5
- Molecular formula:C5H12NOP
- Molecular Weight:133.13
945459-79-0
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Yield:945460-43-5 99%
Reaction Conditions:
with tripotassium phosphate tribasic;ammsnium formate in methanol; for 2 h;Inert atmosphere;Reflux;
Steps:
47 4-methyl-[1,4]azaphosphinane-4-oxide
4-methyl-[1,4]azaphosphinane-4-oxide (0536) A flask was charged with 1-benzyl-4-methyl-[1,4]azaphosphinane-4-oxide (1.00 g, 4.47 mmol) and 10% Pd/C (100 mg). The flask was evacuated and filled with nitrogen. Anhydrous methanol (18 mL) was added to the flask and the flask was equipped with a reflux condenser with a nitrogen inlet. Ammonium formate (2.25 g, 35.8 mmol) was added in one portion at room temperature. The resulting mixture was stirred at reflux for 2 h. The reaction was filtered through a Celite pad and the Celite was washed with 2×5 mL methanol. The combined filtrate and washing was evaporated in vacuo. The crude residue was purified by silica gel chromatography (0-10% 7N ammonia in methanol:dichloromethane) to afford 4-methyl-[1,4]azaphosphinane-4-oxide as a yellow gel (0.589 g, 99% yield).
References:
US2015/225436,2015,A1 Location in patent:Paragraph 0536; 0674
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