Preparation method of 3-ethyl-4-7-aminocephalosporanic acid
A technology of cephalosporanic acid and vinyl, which is applied in the field of preparing 7-amino-3-vinyl-4-cephalosporanic acid, can solve the problems of low equipment requirements, low production cost, high raw material cost, etc., and achieve short reaction route, The effect of less three wastes and low cost of raw materials
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Embodiment 1
[0021] Embodiment 1: Preparation of 7-amino-3-vinyl-4-cephalosporanic acid
[0022] In a 50 ml three-necked flask, add 46 mg (0.1 mmol) of p-methoxybenzyl 7-phenylacetamido-3-vinyl-4-cephalosporanic acid, solid superacid catalyst S 2 o 8 2- / SnO 2 -Fe 2 o 3 23mg, 46mg of dichloromethane, 46mg of isoamyl acetate, 138mg of acetonitrile, react at 5°C for 5 hours, then cool the reaction solution to room temperature, add 10mg of activated carbon to the reaction solution for decolorization, filter, and concentrate the filtrate to precipitate pale yellow The solid was 18.3mg, and the yield was 81%. m.p.180~182℃, purity≥96%.
[0023] IR(KBr)cm -1 : 3158, 3010, 2890, 1800, 1615, 1540, 1060.
[0024] 1 H-NMR (D 2 O,400MHz)δ:3.52~3.67(2H,ABq,C 2 h 2 ),5.02~5.05(1H,dd,C 6 -H),5.19~5.20(1H,dd,C 7 -H), 5.34~5.37 (1H, d, Vinyl-H), 5.38~5.40 (1H, d, Vinyl-H), 6.68~6.72 (1H, dd, Vinyl-H).
Embodiment 2
[0025] Embodiment 2: Preparation of 7-amino-3-vinyl-4-cephalosporanic acid
[0026] In a 50 ml three-necked flask, add 46 mg (0.1 mmol) of p-methoxybenzyl 7-phenylacetamido-3-vinyl-4-cephalosporanic acid, solid superacid catalyst S 2 o 8 2- / SnO 2 -Fe 2 o 3 46 mg, dichloromethane 46 mg, isoamyl acetate 92 mg, acetonitrile 230 mg, react at 0°C for 10 hours, then cool the reaction solution to room temperature, add 10 mg of activated carbon to the reaction solution for decolorization, filter, and concentrate the filtrate to precipitate pale yellow Solid 18.5 mg, yield 82%. m.p.180~182℃, purity≥96%.
Embodiment 3
[0027] Embodiment 3: Preparation of 7-amino-3-vinyl-4-cephalosporanic acid
[0028] In a 50 ml three-necked flask, add 46 mg (0.1 mmol) of p-methoxybenzyl 7-phenylacetamido-3-vinyl-4-cephalosporanic acid, solid superacid catalyst SO 4 2- / SnO 2 -Fe 2 o 3 46mg, 46mg of dichloromethane, 138mg of butyl acetate, 230mg of acetonitrile, react at 0°C for 10 hours, then cool the reaction solution to room temperature, add 10mg of activated carbon to the reaction solution for decolorization, filter, and concentrate the filtrate to precipitate a light yellow solid 18.2 mg, yield 80.6%. m.p.180~182℃, purity≥96%.
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