四丁基碘化膦

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To the autoclave was added 5.81 g (0.022 moles) of Mo(CO)6, 15.5 g (0.040 moles) of tetrabutylphosphonium iodide, 109.2 g (0.700 moles) of ethyl iodide, 555 g (7.5 moles) of propionic acid, and 68.6 g of N-methyl pyrrolidinone (NMP) as polar, aprotic solvent. The condenser temperature is set at 5°-10° C. using a cooled ethylene glycol/water mixture. The autoclave was then pressure tested with nitrogen at 68.0 atm and a gas purge of 3 moles/hr of gas was established through the high pressure condenser. (During the reaction this gas purge permitted control of the gas composition over the reaction mixture and is necessary for kinetic measurements.) The nitrogen was vented, the autoclave was then pressurized to 23.8 atm with 5% hydrogen in carbon monoxide, and subsequently heated to 160° C. (The 3 moles/hr of gas purge is maintained throughout heating and the subsequent reaction.) Upon reaching temperature, the pressure is raised to 51.0 atm using a gas mixture consisting of 6% H2, 47% CO, and 47% ethylene while using the 3 mole/hr purge to maintain the gas mixture. Liquid samples are removed every 20 minutes for 5 hours and analyzed for ethyl iodide, ethyl propionate, propionic anhydride, and propionic acid content by GC using a Hewlett Packard 5890 GC containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard. (A split injection was used to introduce the sample and sample detection was accomplished with TCD detector.) These components represented the only significant products and all other materials detectable by GC-MS were only present at trace levels. Gas samples were also removed hourly and analyzed by GC to insure that the gas mixture is consistent. The molar quantities of propionic anhydride (npan) formed were determined from the GC data using the following equation: ##EQU1## where, ni =moles of the component is set at 5°-10° C. a gas purge of 3 moles/hr of gas (During the reaction this gas purge purge is maintained throughout heating the subsequent reaction the pressure is raised to 51.0 atm purge to maintain the gas mixture Liquid samples are removed every 20 minutes for 5 hours containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard to introduce the sample and sample detection Gas samples were also removed hourly

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To the autoclave was added 5.81 g (0.022 moles) of Mo(CO)6, 15.5 g (0.040 moles) of tetrabutylphosphonium iodide, 109.2 g (0.700 moles) of ethyl iodide, 555 g (7.5 moles) of propionic acid, and 68.6 g of N-methyl pyrrolidinone (NMP) as polar, aprotic solvent. The condenser temperature is set at 5°-10° C. using a cooled ethylene glycol/water mixture. The autoclave was then pressure tested with nitrogen at 68.0 atm and a gas purge of 3 moles/hr of gas was established through the high pressure condenser. (During the reaction this gas purge permitted control of the gas composition over the reaction mixture and is necessary for kinetic measurements.) The nitrogen was vented, the autoclave was then pressurized to 23.8 atm with 5% hydrogen in carbon monoxide, and subsequently heated to 160° C. (The 3 moles/hr of gas purge is maintained throughout heating and the subsequent reaction.) Upon reaching temperature, the pressure is raised to 51.0 atm using a gas mixture consisting of 6% H2, 47% CO, and 47% ethylene while using the 3 mole/hr purge to maintain the gas mixture. Liquid samples are removed every 20 minutes for 5 hours and analyzed for ethyl iodide, ethyl propionate, propionic anhydride, and propionic acid content by GC using a Hewlett Packard 5890 GC containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard. (A split injection was used to introduce the sample and sample detection was accomplished with TCD detector.) These components represented the only significant products and all other materials detectable by GC-MS were only present at trace levels. Gas samples were also removed hourly and analyzed by GC to insure that the gas mixture is consistent. The molar quantities of propionic anhydride (npan) formed were determined from the GC data using the following equation: ##EQU1## where, ni =moles of the component is set at 5°-10° C. a gas purge of 3 moles/hr of gas (During the reaction this gas purge purge is maintained throughout heating the subsequent reaction the pressure is raised to 51.0 atm purge to maintain the gas mixture Liquid samples are removed every 20 minutes for 5 hours containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard to introduce the sample and sample detection Gas samples were also removed hourly

反应条件: temp:180.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: As in Example 1, 1,3-hexadiene (0.99 g, 12.06 mmol), trichlorosilane (6.60 g, 48.73 mmol) and tetrabutylphosphonium iodide (0.47 g, 1.22 mmol) were added in a 25 mL stainless steel tube under nitrogen atmosphere. After sealing the cylinder with a cap, the reactor was maintained at 180 ° C. for 10 hours. The resulting mixture was distilled to yield 1.32 g (yield: 60%) of 1,1-dichloro-2,5-dimethyl-silacyclo-3-pentene and 0.43 g (yield: 10%) of 2,5-bis(trichlorosilyl)-3-hexene main products. The resulting mixture was distilled

反应条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To the autoclave was added 5.81 g (0.022 moles) of Mo(CO)6, 15.5 g (0.040 moles) of tetrabutylphosphonium iodide, 109.2 g (0.700 moles) of ethyl iodide, 555 g (7.5 moles) of propionic acid, and 68.6 g of N-methyl pyrrolidinone (NMP) as polar, aprotic solvent. The condenser temperature is set at 5°-10° C. using a cooled ethylene glycol/water mixture. The autoclave was then pressure tested with nitrogen at 68.0 atm and a gas purge of 3 moles/hr of gas was established through the high pressure condenser. (During the reaction this gas purge permitted control of the gas composition over the reaction mixture and is necessary for kinetic measurements.) The nitrogen was vented, the autoclave was then pressurized to 23.8 atm with 5% hydrogen in carbon monoxide, and subsequently heated to 160° C. (The 3 moles/hr of gas purge is maintained throughout heating and the subsequent reaction.) Upon reaching temperature, the pressure is raised to 51.0 atm using a gas mixture consisting of 6% H2, 47% CO, and 47% ethylene while using the 3 mole/hr purge to maintain the gas mixture. Liquid samples are removed every 20 minutes for 5 hours and analyzed for ethyl iodide, ethyl propionate, propionic anhydride, and propionic acid content by GC using a Hewlett Packard 5890 GC containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard. (A split injection was used to introduce the sample and sample detection was accomplished with TCD detector.) These components represented the only significant products and all other materials detectable by GC-MS were only present at trace levels. Gas samples were also removed hourly and analyzed by GC to insure that the gas mixture is consistent. The molar quantities of propionic anhydride (npan) formed were determined from the GC data using the following equation: ##EQU1## where, ni =moles of the component is set at 5°-10° C. a gas purge of 3 moles/hr of gas (During the reaction this gas purge purge is maintained throughout heating the subsequent reaction the pressure is raised to 51.0 atm purge to maintain the gas mixture Liquid samples are removed every 20 minutes for 5 hours containing a 25 m (0.25 mm ID, 0.25 micron film) Quadrex 007 FFAP Capillary Column with p-xylene as an internal standard to introduce the sample and sample detection Gas samples were also removed hourly