Preparation method of polyfluoro aliphatic carboxylic acid
A technology of aliphatic carboxylic acid and fluorine-containing carboxylic acid potassium salt, which is applied in the synthesis of polyfluoroaliphatic carboxylic acid surface-active compounds and in the field of polyfluoroaliphatic carboxylic Low yield and other problems, to achieve the effect of less reaction by-products, high yield, easy to purify
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Embodiment 1
[0020] Synthesis of 2,2,3,3,4,4,5,5-octafluoropentanoic acid:
[0021] 116.0 g of 2, 2, 3, 3, 4, 4, 5, 5-octafluoropentanol, 700 g of water, and 200 g of acetic acid were sequentially added to a 2 L three-necked flask. Stir and heat up to 80°C, add 126.4 g of potassium permanganate three times, and keep the reaction for 4 hours. Cool to room temperature and filter to obtain a colorless transparent filtrate. The filtrate was washed three times with 300 g of ethyl acetate, then acidified with concentrated hydrochloric acid to pH = 2, extracted three times with 750 g of ethyl acetate, washed with water, added with 12 g of anhydrous sodium sulfate, dried for 1 hour, filtered to remove the desiccant, and concentrated to obtain The crude product was rectified to obtain 96.0 g of the product 2,2,3,3,4,4,5,5-octafluoropentanoic acid, and its purity was 98.5% as determined by gas chromatography. Yield 78.0%. Product IR v: 3219.8 (-COOH), 2997.4 (H-CF 2 ), 1776.1 (C=O), 1181.8, 1078...
Embodiment 2
[0023] 116.0 g of 2, 2, 3, 3, 4, 4, 5, 5-octafluoropentanol, 700 g of water, and 200 g of acetic acid were sequentially added to a 2 L three-necked flask. Stir and heat up to 80°C, add 142.2 g of potassium permanganate three times, and keep the reaction for 4 hours. Cool and filter to obtain a colorless transparent filtrate. The filtrate was washed three times with 300g of dichloromethane, then acidified with concentrated hydrochloric acid to pH = 2, extracted three times with 750g of dichloromethane, washed with water, dried by adding 10g of anhydrous magnesium sulfate, filtered to remove the desiccant for 30 minutes, and the filtrate was concentrated The crude product was obtained, and 104.6 g of product 2,2,3,3,4,4,5,5-octafluoropentanoic acid was obtained by rectification, and its purity was 98.0% as determined by gas chromatography. Yield 85.1%.
Embodiment 3
[0025] 116.0 g of 2, 2, 3, 3, 4, 4, 5, 5-octafluoropentanol, 700 g of water, and 200 g of acetic acid were sequentially added to a 2 L three-necked flask. Stir and heat up to 90°C, add 158.0 g of potassium permanganate three times, and keep the reaction for 5 hours. Cool and filter to obtain a colorless transparent filtrate. The filtrate was washed three times with 300g of dichloroethane, then acidified with concentrated hydrochloric acid to pH = 2, extracted three times with 750g of dichloroethane, washed with water, added with 12g of anhydrous sodium sulfate to dry for 2 hours, filtered to remove the desiccant, The filtrate was concentrated to obtain a crude product, which was rectified to obtain 111.4 g of the product 2,2,3,3,4,4,5,5-octafluoropentanoic acid with a purity of 98.7% as determined by gas chromatography. Yield 90.6%.
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