ChemicalBook CAS DataBase List PINOXADEN

PINOXADEN synthesis

6synthesis methods

Product Name:PINOXADEN
CAS Number:243973-20-8
Molecular formula:C23H32N2O4
Molecular Weight:400.51

314020-44-5 Synthesis

314020-44-5
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3282-30-2
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243973-20-8
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$210.00/2.5mg

Yield:243973-20-8 93.98%

Reaction Conditions:

with dmap;triethylamine in tetrahydrofuran at 0 - 25; for 1.5 h;

Steps:

1.3; 2.3; 3.3
(3)60g of tetrahydrofuran,15.4g 8- (2,6-diethyl-4-methylbenzene) -1,2,4,5-tetrahydropyrazole [1,2-d] [1,4,5] oxodiazepine- 7,9-dione (molecular weight 316.4, 48.67 mmol, 1.0 eq),24.62g of triethylamine (molecular weight 101.19, 146.0 mmol, 5.0 eq)And 297.3 mg DMAP (Molecular weight 122.17, 2.43 mmol, 0.05 eq),Cool down to 0 ,Slowly add 7.63 g of pivaloyl chloride (molecular weight 120.58, 63.27 mmol, 1.3 eq),White turbidity was formed during the dropwise addition. After dripping, stir for 0.5h, then transfer to room temperature and stir at 25 ° C for 1h.Add 100g of water to dilute,Extracted twice with 100 mL of ethyl acetate,Combined organic phases,The organic phase was distilled off under reduced pressure to obtain a crude product.The crude product was recrystallized from methyl tert-butyl ether to obtain 18.39 g.(Molecular weight: 400.52, theoretical yield: 19.49 g) White solid. The purity measured by HPLC is 99.6%, which is pinoxaden, with a mass yield of 93.98%.

References:

Jiangsu Zhongqi Technology Co., Ltd.;Bu Long;Wu Yaojun;Zhang Pu;Hou Yuanchang CN110294768, 2019, A Location in patent:Paragraph 0031; 0034; 0035; 0038; 0039; 0042

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