A kind of synthetic method of telamycin A
A telamycin and synthesis method technology, applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., can solve the problems of long reaction time, many unsafe factors, large amount of catalyst palladium carbon, etc., and achieve simple operation Safer, avoiding hydrogenation reaction, and improving reaction efficiency
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Embodiment 1
[0035]Put 20 g of epoxide (compound 2), 80 g of isopropanol and 20 g of n-propylamine into a 250 mL three-necked flask, start stirring, and react at 20 °C after the dissolution is complete, and react at 20 °C for 48 h. Add 60 g of methylamino alcohol solution into the reaction bottle, and react at 40 °C for 24 h, and the reaction is monitored by HPLC. After the reaction finishes, all solvents and excess deprotection reagents are distilled off under reduced pressure, and 100 g of methyl tert-butyl ether is added to the residue, stirred and dissolved completely, and 6.1 g of trifluoroacetic acid and 60 g of methyl tert-butyl ether are added dropwise. The mixture was stirred for 4 h, filtered, and dried to obtain the trifluoroacetic acid salt of telamycin. Add 140 mL of dichloromethane to the trifluoroacetic acid salt, add potassium carbonate aqueous solution (potassium carbonate 8.93 g, water 140 mL) under stirring, and separate layers after stirring for 30 min, add 140 mL of di...
Embodiment 2
[0037] Put 20 g of epoxide (compound 2), 80 g of n-butanol and 30 g of n-propylamine into a 250 mL three-necked flask, start stirring, and heat up the oil bath to the internal temperature of 40 °C after the dissolution is complete, and react at 40 °C for 24 h. Add 60 g of methylamine aqueous solution to the reaction bottle, and react at 40 °C for 24 h, and the reaction is monitored by HPLC. After the reaction was completed, all solvents and excess deprotection reagents were distilled off under reduced pressure, and 100 g of ethanol was added to the residue, stirred and dissolved completely, and a mixture of 6.1 g of phosphoric acid and 60 g of methyl tert-butyl ether was added dropwise, and stirred for 4 h. Filter and dry to obtain the phosphate of telamycin. Add 140 mL of dichloromethane to the phosphate, add potassium carbonate aqueous solution (8.93 g of potassium carbonate, 140 mL of water) while stirring, and separate layers after stirring for 30 min, add 140 mL of dichl...
Embodiment 3
[0039] Put 20 g of epoxide (compound 2), 100 g of methanol and 30 g of n-propylamine into a 250 mL three-necked flask, start stirring, and after the dissolution is complete, heat the oil bath to an internal temperature of 30 °C, and react at 30 °C for 24 h. Add 40 g of methylethylamine solution into the reaction bottle, and react at 30 °C for 12 h, and the reaction is monitored by HPLC. After the reaction finishes, all solvents and excess deprotection reagents are distilled off under reduced pressure, and 100 g of methyl tert-butyl ether is added to the residue, stirred and dissolved completely, and 6.1 g of trifluoroacetic acid and 60 g of methyl tert-butyl ether are added dropwise. The mixture was stirred for 4 h, filtered, and dried to obtain the trifluoroacetic acid salt of telamycin. Add 140 mL of dichloromethane to the trifluoroacetic acid salt, add potassium carbonate aqueous solution (potassium carbonate 8.93 g, water 140 mL) under stirring, and stir for 30 minutes, th...
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