ChemicalBook CAS DataBase List 3,5,6-Trichloro-2-pyridinol

3,5,6-Trichloro-2-pyridinol synthesis

7synthesis methods

Product Name:3,5,6-Trichloro-2-pyridinol
CAS Number:6515-38-4
Molecular formula:C5H2Cl3NO
Molecular Weight:198.43

2402-79-1

6515-38-4

The general procedure for the synthesis of 3,5,6-trichloropyridin-2(1H)-one from 2,3,5,6-tetrachloropyridine: 2,3,5,6-tetrachloropyridine 43.4g (0.2 mol) and 240mL of deionized water were added into a three-necked flask, and the temperature was raised to 95℃ under stirring. Subsequently, 39.53 g (0.60 mol, 85% purity) of potassium hydroxide was slowly added and the pH of the reaction solution was adjusted to 9.5~10. Stirring was maintained at this temperature for 30 min, and the reaction was completed by filtration while hot to remove insoluble impurities. The filtrate was transferred to a 500 mL autoclave and 0.18 g of potassium hydroxide and benzyltrimethylammonium chloride were added as phase transfer catalyst. The autoclave was sealed, the reaction mixture was stirred and heated to 120 °C and kept at this temperature for 4.0 hours. At the end of the reaction, the reaction was cooled to 25 °C and the pH was adjusted to 4.0~4.5 with 15% hydrochloric acid solution. the reaction mixture was filtered and the resulting solid was washed with deionized water and dried to give 35.9 g of a white powdery product 3,5,6-trichloropyridin-2(1H)-one. The purity of the product was 99.08% by gas chromatography.

2402-79-1 Synthesis

2402-79-1
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$5.00/1g

6515-38-4
164 suppliers
$9.00/1g

Yield:6515-38-4 87%

Reaction Conditions:

with tetrabutylammomium bromide;sodium hydroxide in water at 100; for 8 h;Inert atmosphere;

Steps:

General procedure for intermediate F.
2,3,5,6-Tetrachloropyridine (0.1 mol), NaOH, TBAB and 60mL H2O were added to a 100 mL eggplant-shaped. The mixture was heated at 100 °C for 8 hours, and monitored by TLC. Upon the reaction completion, the mixture was poured into icewater (100 mL) and was acidified to pH = 5-6. After filtration and extraction, F was obtained as white solid. The analytical data corresponded to the literature [15, 16].

References:

Huang, Hao;Liu, Jian-Min;Shu, Lei;Wang, Man-Man;Yan, Yi-Le;Zhang, Da-Yong;Zhang, Jian-Qiu [Beilstein Journal of Organic Chemistry,2020,vol. 16,p. 233 - 247] Location in patent:supporting information

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