Composition containing chloromethyl phosphate derivative with improved stability and method for producing the same
A composition and compound technology, which can be applied to phosphorus organic compounds, compounds of Group 5/15 elements of the periodic table, chemical instruments and methods, etc. The problems of unrealistic industrial preparation methods, etc., to achieve the effect of stabilization and energy saving
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preparation example 1
[0093] Synthesis of Chloromethyl Chlorosulfonate
[0094]
[0095] Add paraformaldehyde (10 g) into a 100 mL four-necked flask, and stir in an ice-water bath. Chlorosulfonic acid (24 mL) was added dropwise at an internal temperature of below 80°C, and after stirring at room temperature for 1 hour, thionyl chloride (22 mL) was added dropwise. After completion of the dropping, heating was performed at 60° C. for 3 hours, followed by cooling. The reaction solution was dropped into ice water (400 mL), followed by liquid separation. After washing with water, MgSO was added to the organic layer 4 , diluted with hexane equivalent to the organic layer, filtered to remove MgSO 4 . The filtrate was concentrated under reduced pressure, and the resulting residue was distilled under reduced pressure to obtain 15 g of the title compound as a colorless and transparent liquid. (BP50~60°C / 18~20mmHg) (30% yield).
preparation example 2
[0097] Synthesis of Chloromethyl Chlorosulfonate
[0098]
[0099] Add paraformaldehyde (10 g) into a 200 mL four-necked flask, and stir in an ice-water bath. Thionyl chloride (22 mL) was added dropwise, followed by chlorosulfonic acid (24 mL). After stirring at room temperature for 4 hours, it was heated at 60°C for 14 hours and cooled. The reaction solution was dropped into ice water (400 mL) for liquid separation. After washing with water, MgSO was added to the organic layer 4 , diluted with an equal amount of hexane to the organic layer, and filtered. After concentration under reduced pressure, the resulting residue was distilled under reduced pressure to obtain 7.9 g of the title compound as a colorless and transparent liquid. (BP 54°C / 15mmHg) (Yield 16%)
Embodiment 1
[0101] Synthesis of Di-tert-butyl Chloromethyl Phosphate
[0102]
[0103] Install a mechanical stirrer and a thermometer on a 2L four-neck round bottom flask, add di-tert-butyl potassium phosphate (100g), dipotassium hydrogen phosphate (561.2g), tetrabutyl ammonium hydrogen sulfate (13.7g), tert-butyl methyl ether (400mL) and water (700mL), stirring while cooling in a water bath. At an internal temperature of 28°C or lower, chloromethyl sulfonate (99.7 g) having an internal temperature of 23°C was added dropwise over 2 hours. After the dropwise addition, the mixture was stirred for 2 hours, water (300 mL) was added, the lower layer was separated, and the organic layer was washed with 5N aqueous sodium hydroxide solution (600 mL) and 2M aqueous solution of potassium hydrogen phosphate (600 mL). N,N-Diisopropylethylamine (10.4 g) was added to the organic layer, followed by washing with water (200 mL). N,N-diisopropylethylamine (10.4 g) was added, and after washing with wat...
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Abstract
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