1,3,4-Thiadiazol-2-aMine, 5-[(4-chlorophenoxy)Methyl]- synthesis
- Product Name:1,3,4-Thiadiazol-2-aMine, 5-[(4-chlorophenoxy)Methyl]-
- CAS Number:84138-73-8
- Molecular formula:C9H8ClN3OS
- Molecular Weight:241.7
122-88-3
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Yield:84138-73-8 96.2%
Reaction Conditions:
with silica gel;trichlorophosphate at 20; for 0.166667 h;
Steps:
4
1) was added 0.05mol thiosemicarbazide To a dry mortar, 0.055 mol phenoxyacetic acid, phosphorus oxychloride and 0.055 mol 0.25mol silica abrasive 10min at room temperature at which time TLC monitoring showed starting material disappeared thiosemicarbazide point, indicates complete reaction of starting material, then allowed to stand 30min, to obtain a crude product; TLC developing solvent wherein the volume ratio of 1: 3 mixture of ethyl acetate and petroleum ether; document.write("");2) The crude product was transferred to a beaker, was added to the crude product concentration of 5% sodium carbonate solution, pH of the resulting mixture to a value of 8, and then the mixture is filtered off with suction, the resulting cake with a solvent DMF after dissolution continued suction filtration, silica gel was removed, and then the resulting filtrate was concentrated under reduced pressure, the solvent was removed, and then concentrated under reduced pressure to give the product washed with water, filtered off with suction, i.e. 2-amino-5-phenoxy-methylene -1 , 3,4-thiadiazole, in a yield of 91.3%.
References:
CN103880776,2016,B Location in patent:Paragraph 0036-0038
119869-03-3
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84138-73-8
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106-48-9
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14426-42-7
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2381-75-1
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84138-73-8
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