Pyran fluorinated compound, preparation method and application of pyran fluorinated compound
A compound and pyran-based technology, applied in the field of pyran-based compounds and their synthesis, can solve the problems of uncontrollable properties and few types of compounds, and achieve the effects of simple synthesis methods, expanded types, and broad application prospects
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0031] The synthesis of embodiment 1 compound (1)
[0032]
[0033] 1. Synthesis
[0034] Add 0.21mol CeCl to a 2L dry and clean three-neck flask 3 , 200ml THF, nitrogen protection, temperature control to 35 ℃ ~ 40 ℃ for 1 hour to react; 0.27mol magnesium chips, 10ml THF, 0.1g iodine and a small amount of Stir to initiate the reaction, and add the remaining and 500ml of THF, react at a temperature of about 25°C for 1.5 hours for later use; at a temperature of about 5°C, add 0.25mol of the Grignard reagent obtained above to the prepared CeCl 3 In THF solution, react for 1 hour; control temperature -5℃~0℃, add 0.19mol dropwise And 100ml of THF solution, dropwise temperature control reaction for 1 hour. Slowly pour the reaction solution into a beaker filled with crushed ice and 100ml of concentrated hydrochloric acid, acidify and hydrolyze, separate the liquids after stirring, extract the aqueous phase twice with 50ml×2 toluene, combine the organic phases, wash the or...
Embodiment 2
[0044] The synthesis of embodiment 2 compound (2)-(9)
[0045] Synthesize other part monofluoro compounds with different starting materials, with the same method of embodiment 1:
[0046]
[0047] Mass spectrometry: 298 (molecular ion peak), 278 (losing one HF);
[0048] Elemental analysis: C 76.42%, H 11.79%, F 6.35%, O 5.35%.
[0049] 1 HNMR(CDCl3,300MHz)δ H : 0.85~1.62(m,30H), 1.90~2.12(m,1H), 3.30~3.41(m,1H), 3.54~3.60(m,3H).
[0050]
[0051] Mass spectrometry: 254 (molecular ion peak), 234 (losing one HF);
[0052] Elemental analysis: C 74.90%, H 11.29%, F 7.48%, O 6.31%.
[0053] 1 HNMR(CDCl3,300MHz)δ H :0.85~1.62(m,18H), 1.95~2.32(m,2H), 3.30~3.62(m,4H), 4.90~5.10(m,2H), 5.65~5.71(m,1H).
[0054]
[0055] Mass spectrometry: 282 (molecular ion peak), 262 (losing one HF);
[0056] Elemental analysis: C 76.57%, H 10.97%, F 6.73%, O 5.65%.
[0057] 1 HNMR(CDCl3,300MHz)δ H : 0.85~1.62(m,22H), 1.95~2.32(m,2H), 3.30~3.62(m,4H), 4.90~5.10(m,2H), 5.71~5.83(...
Embodiment 3
[0078] The synthesis of embodiment 3 compound (10)
[0079]
[0080] Prepared with Example 1 as the starting material.
[0081] 1. Synthesis
[0082] Add 300ml of water and 21ml of concentrated sulfuric acid (98%) into a 1L three-necked flask, stir, cool the ice water to about 10°C, and add 0.22mol 75ml of acetone and 130ml of dichloromethane were added and stirred for 5 minutes. Add 0.28mol potassium permanganate in batches at a temperature controlled below 20°C, and react for 2 hours at a temperature controlled at 15°C-20°C after adding. Slowly pour the reaction solution into a saturated aqueous solution of sodium bicarbonate, stir and separate the liquids, and use 50ml×2 CH for the aqueous phase 2 Cl 2 Extracted twice, combined the organic phases, washed twice with 100ml×2 saturated NaCl aqueous solution, dried over anhydrous sodium sulfate, spin-dried the solvent, passed through a silica gel column, spin-dried the solvent and crystallized with ethanol to obtain...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More