Best Manufacturing Methods for Pest Control Agents
一种制造方法、化合物的技术,应用在植物学设备和方法、杀生剂、动物驱避剂等方向,能够解决不适合工业制造等问题,达到高收率的效果
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Embodiment 1
[0070] Add 31.24g (0.22mol) of ethyl trifluoroacetate, 18.82g (0.20mol) of 2-aminopyridine, and 16g of N,N-dimethylformamide (DMF) in sequence, and add sodium methoxide (28.0% methanol solution) 38.57g (0.20mol). After stirring at 25° C. for 1 hour, methanol and ethanol were distilled off under reduced pressure. What dissolved 32.70 g (0.20 mol) of 2-chloro-5-chloromethylpyridine in 18.8 g of DMF was added there, and it stirred at 60 degreeC for 3 hours and 15 minutes. Then, 110 ml of water was added, and after stirring at room temperature for 3 hours, the precipitate was collected by filtration, pressure-washed twice with 40 ml of water, and 59.81 g of the target object (94.7% yield, purity 98.6%).
Embodiment 2~4 and comparative example 1
[0072] In Examples 2-4, as shown in Table 1, change the ethyl trifluoroacetate of step 1 in Example 1 relative to the equivalent of 2-aminopyridine to carry out the reaction, and obtain the yield and purity shown in Table 1. Target. In Comparative Example 1, the reaction was carried out by changing the equivalent of ethyl trifluoroacetate to 1 equivalent of 2-aminopyridine in Step 1 in Example 1 as shown in Table 1. As a result, although the target object was obtained, as shown in Table 1, it was an inferior result compared with the yield of Examples 1-4.
[0073]
Embodiment 5~7 and comparative example 2 and 3
[0075] In Examples 5 to 7, as shown in Table 2, change the sodium methylate of Step 1 in Example 1 relative to 1 equivalent of 2-aminopyridine to carry out the reaction, and obtain the yield and purity targets shown in Table 2. thing. In Comparative Examples 2 and 3, the reaction was carried out by changing the equivalent of sodium methoxide to 1 equivalent of 2-aminopyridine in Step 1 in Example 1 as shown in Table 2. As a result, although the target object was obtained, as shown in Table 2, it was an inferior result compared with the yield of Example 1, 5-7.
[0076]
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