Compounds containing naphthyl substituted pyridazine structural unit, and preparation method and application thereof
A compound and a technology for preparation steps are applied in the field of new compounds containing naphthyl-substituted pyridazine structural units and their preparation fields, and can solve problems such as the gap between practical applications and the like
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Embodiment 1
[0080] Embodiment 1, compound preparation of
[0081] step 1: Synthesis
[0082]
[0083] Into the 250mL reaction flask, put 58.1mmol of 2-naphthoic acid and 40mL of ethanol, then heat to reflux, add 2mL of thionyl chloride dropwise, and reflux for 6 hours after the dropwise addition. Then the reaction solution was spin-dried to obtain a colorless liquid product, yield: 90%.
[0084] Step 2: Synthesis
[0085]
[0086] Into a 250mL reaction flask, put 52.4mmol of compound 1a obtained in Step 1 of Example 1, 104.8mmol of NaH and 100mL of THF, and heat to maintain reflux. A solution of 78.7 mmol ethyl acetate in 30 mL THF was added dropwise, and after the dropwise addition was completed, the reaction was refluxed for 8 hours. Add 100ml of saturated aqueous solution of sodium chloride and 50mL of ethyl acetate to the system, stir and separate the liquids, extract the aqueous phase twice with 30mL of ethyl acetate, wash the organic phase twice with 30mL of saturat...
Embodiment 2
[0117] Embodiment 2, compound Synthesis
[0118] Step 1-step 7 is the same as embodiment 1.
[0119] Step 8: Synthesis
[0120]
[0121] In this step, referring to step 8 of Example 1, the methyl bromide in Step 8 of Example 1 was replaced with bromobenzene, and other operations were the same as Step 8 of Example 1 to prepare the target compound with a yield of 66%.
[0122] Step 9: Synthesis
[0123]
[0124] For this step, refer to step 9 of Example 1, replace 1h in step 9 of Example 1 with compound 2h obtained in step 8 of Example 2, and other operations are the same as step 9 of Example 1 to prepare the target compound, yield: 58% .
[0125] Step 10: Synthesis
[0126]
[0127] This step refers to step 10 of Example 1, replaces 1i in step 10 of Example 1 with compound 2i obtained in step 9 of Example 2, and other operations are the same as step 10 of Example 1 to prepare the target compound, yield: 71% .
[0128] 1 H NMR (CDCl 3,300MHz): δ=8.76...
Embodiment 3
[0134] Embodiment 3, compound Synthesis
[0135] step 1: Synthesis
[0136]
[0137] This step refers to step 1 of Example 1, and the 2-naphthoic acid in step 1 of Example 1 is replaced by 1-methyl 2-naphthoic acid, and other operations are the same as step 1 of Example 1 to prepare the target compound. The yield : 92%.
[0138] Step 2: Synthesis
[0139]
[0140] For this step, refer to step 2 of Example 1, replace 1a in step 2 of Example 1 with compound 3a obtained in step 1 of Example 3, and other operations are the same as step 2 of Example 1 to prepare the target compound, yield: 86% .
[0141] Step 3: Synthesis
[0142]
[0143] For this step, refer to step 3 of Example 1, replace 1b in step 3 of Example 1 with compound 3b obtained in step 2 of Example 3, and other operations are the same as step 3 of Example 1 to prepare the target compound, yield: 77% .
[0144] Step 4: Synthesis
[0145]
[0146] This step refers to step 4 of Example ...
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