Ethyl triphenyl phosphonium chloride preparation method
A technology of ethyl triphenyl phosphine chloride and triphenyl phosphine, applied in the field of preparation of ethyl triphenyl phosphine chloride, can solve the problem of low purity, low yield of ethyl triphenyl phosphine chloride, etc. question
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Embodiment 1
[0018] A preparation method of ethyltriphenylphosphine chloride:
[0019] Weigh 1mol of triphenylphosphine and 8.5mol of acetonitrile, put them into a 2000L pressure reactor, then add 1.0mol of ethyl chloride dropwise, seal the reactor after the dropwise addition; open the steam inlet valve for heating , the temperature in the pressure reactor is controlled to be 120°C, and the pressure in the kettle is 10kg / cm 2 , and keep warm for 35 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 50°C, vent the pressure reactor, keep warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.5%, and keep the supernatant for later use; the precipitate after centrifugation After drying at 100°C for 10 hours, 0....
Embodiment 2
[0021] Weigh 1mol of triphenylphosphine and 5mol of acetonitrile, put them into a 2000L pressure reactor, add 1.2mol of ethyl chloride dropwise, seal the reactor after the addition is complete; open the steam inlet valve for heating, Control the temperature in the pressure reactor to 140°C, and the pressure in the kettle to 11kg / cm 2 , and keep it warm for 32 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 55°C, vent the pressure reactor, keep it warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.8%, and keep the supernatant for later use; the precipitate after centrifugation After drying at 105°C for 18 hours, 0.9498 mol of triphenylphosphine was obtained with a yield of 94.98%. The puri...
Embodiment 3
[0023] Weigh 1mol of triphenylphosphine and 10mol of acetone, put them into a 2000L pressure reactor, then add 1.5mol of ethyl chloride dropwise, seal the reactor after the addition; open the steam inlet valve for heating, Control the temperature in the pressure reactor to 150°C, and the pressure in the kettle to 12kg / cm 2 , and keep it warm for 40 hours; then close the steam inlet valve, feed cooling water to cool down the pressure reactor, cool down to 60°C, vent the pressure reactor, keep it warm for 1 hour, recover and exhaust the unreacted ethyl chloride, and return to Atmospheric pressure, continue to cool down to room temperature; then centrifuge the reacted product in the reactor, test the water content of the supernatant after centrifugation, the water content is 4.8%, and keep the supernatant for later use; the precipitate after centrifugation Dry at 105°C for 18 hours, then mix with acetonitrile, heat and reflux, cool and crystallize, and centrifuge for 48 hours, th...
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