1/20 water-containing furosemide compound and preparation method thereof
A furosemide and compound technology, applied in the field of 1/20 water furosemide compounds and preparation methods, can solve the problems of poor stability, easy moisture absorption, low purity and the like, and achieve the effects of good stability, not easy to absorb moisture, and high purity
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Embodiment 1
[0038] The preparation of embodiment 1 1 / 20 water furosemide compound
[0039] (1) 150.73 g of 4-chloro-2-[(furan-2-methyl)-amino]-5-sulfonamidobenzoic acid methyl ester was dissolved in 1.5 L of ethanol, and then 150 ml of 20% aqueous sodium hydroxide solution was added, React at room temperature. After the reaction, adjust the pH to 6.5 with 3 mol / L hydrochloric acid, concentrate to dryness under pressure, and dry under reduced pressure at 45°C for 30 minutes to obtain 113.7 g of crude furosemide, with a yield of 78.7%.
[0040] (2) 113g of furosemide crude product was dissolved in 578.2g of ethyl acetate to make 20% ethyl acetate solution;
[0041] (3) Cool down to room temperature, gradually precipitate crystals, let stand for 4 hours, filter, and wash with ethanol;
[0042] (4) The filtered crystals were dried under reduced pressure at 45° C. for 40 min to obtain 96.54 g of furosemide compound with a yield of 85.4%.
Embodiment 2
[0043] The preparation of embodiment 2 1 / 20 furosemide water compound
[0044] (1) 142.3 g of 4-chloro-2-[(furan-2-methyl)-amino]-5-sulfonamidobenzoic acid methyl ester was dissolved in 1.4L of ethanol, and then 140 ml of 20% aqueous sodium hydroxide solution was added, React at room temperature. After the reaction, adjust the pH to 7.0 with 3 mol / L hydrochloric acid, concentrate to dryness under pressure, and dry under reduced pressure at 45°C for 30 minutes to obtain 109.4 g of crude furosemide, with a yield of 79.3%.
[0045] (2) 109 g of furosemide crude product was dissolved in 321.8 g of ethyl acetate to make 35% ethyl acetate solution;
[0046](3) Cool down to room temperature, gradually precipitate crystals, let stand for 2 hours, filter, and wash with ethanol;
[0047] (4) The filtered crystals were dried under reduced pressure at 38° C. for 50 min to obtain 93.88 g of furosemide compound with a yield of 86.1%.
Embodiment 3
[0048] The preparation of embodiment 3 1 / 20 furosemide water compound
[0049] (1) 160.1 g of 4-chloro-2-[(furan-2-methyl)-amino]-5-sulfonamidobenzoic acid methyl ester was dissolved in 1.6L of ethanol, and then 160 ml of 20% aqueous sodium hydroxide solution was added, React at room temperature. After the reaction, adjust the pH to 7.5 with 3 mol / L hydrochloric acid, concentrate to dryness under pressure, and dry under reduced pressure at 45°C for 30 minutes to obtain 132.9 g of crude furosemide, with a yield of 79.9%.
[0050] (2) 132g of furosemide crude product was dissolved in 452.1g ethyl acetate to make 30% ethyl acetate solution;
[0051] (3) cool down to room temperature, gradually precipitate crystals, let stand for 3 hours, filter, and wash with ethanol;
[0052] (4) The filtered crystals were dried under reduced pressure at 50° C. for 30 minutes to obtain 116.79 g of furosemide compound with a yield of 88.5%.
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