Improved technology for condensation reaction in propiconazole synthesis
A technology of condensation reaction and propiconazole is applied in the field of improved technology of condensation reaction in the synthesis of propiconazole, can solve the problems of long condensation reaction time, difficult solvent treatment, dehydration difficulty and the like, avoids difficulty in solvent recovery, shortens dehydration and the like. time, and the effect of reducing energy consumption
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0028] A kind of improved technology of condensation reaction in the synthesis of propiconazole
[0029] Including the following steps:
[0030] S1. Add 239㎏ triazole and 201㎏ potassium hydroxide into the 3000L reactor, then cover the manhole cover, raise the temperature at a rate of 1.5°C / min while stirring at a rate of 350 rpm, when the temperature rises to 58°C Finally, turn on the vacuum, the vacuum degree is -0.098MPa, and dehydrate under reduced pressure. When the temperature rises to 138°C, continue to dehydrate for 2 hours, then cool down to 70°C, add 990㎏ bromide, 1450㎏DMF, and then open the steam to raise the temperature to 140 ℃, heat preservation reaction for 5.5 hours, control in the sampling, control the bromide content to 0.08%, and the reaction is over;
[0031] Among the above, the bromide is trans-2-bromomethyl-2-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane.
[0032] S2. After the reaction is over, after recovering DMF under reduced pressure at a temperature...
Embodiment 2
[0034] A kind of improved technology of condensation reaction in the synthesis of propiconazole
[0035] Including the following steps:
[0036] S1. Add 259kg of triazole and 221kg of potassium hydroxide into a 3000L reactor, then cover the manhole cover, raise the temperature at a rate of 3.5°C / min while stirring at a rate of 650 rpm, when the temperature rises to 62°C Finally, turn on the vacuum, the vacuum degree is -0.092MPa, and dehydrate under reduced pressure. When the temperature rises to 142°C, continue to dehydrate for 3 hours, then cool down to 80°C, add 1010㎏ bromide, 1550㎏DMF, and then open the steam to raise the temperature to 145 ℃, heat preservation reaction for 6 hours, control in the sampling, control the bromide content to 0.12%, and the reaction is over;
[0037] Among the above, the bromide is trans-2-bromomethyl-2-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane.
[0038] S2. After the reaction is over, after recovering DMF under reduced pressure at a temper...
Embodiment 3
[0040] A kind of improved technology of condensation reaction in the synthesis of propiconazole
[0041] Including the following steps:
[0042] S1. Add 245kg of triazole and 206kg of potassium hydroxide into a 3000L reactor, then cover the manhole cover, raise the temperature at a rate of 2.0°C / min while stirring at a rate of 450 rpm, when the temperature rises to 59°C Finally, turn on the vacuum, the vacuum degree is -0.093MPa, and dehydrate under reduced pressure. When the temperature rises to 139°C, continue to dehydrate for 2.2 hours, then cool down to 72°C, add 995㎏ bromide, 1470㎏DMF, and then open the steam to raise the temperature to 141 ℃, heat preservation reaction for 5.6 hours, control in the sampling, control the bromide content to 0.20%, and the reaction is over;
[0043] Among the above, the bromide is trans-2-bromomethyl-2-(2,4-dichlorophenyl)-4-propyl-1,3-dioxolane.
[0044]S2. After the reaction is over, after recovering DMF under reduced pressure at a temp...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More