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ChemicalBook CAS DataBase List Amlodipine Besylate
111470-99-6

Amlodipine Besylate synthesis

10synthesis methods
-

Yield:111470-99-6 91.6%

Reaction Conditions:

Stage #1: 4-(2-chlorophenyl)-3-ethoxycarbonyl-5-methoxycarbonyl-6-methyl-2-[2-phthalimidoethoxymethyl]-1,4-dihydropyridinewith methylamine at 25;Large scale;
Stage #2: benzenesulfonic acid in water at 30;Large scale;Temperature;

Steps:

1.6; 1.7; 1.8; 13; 14; 15.7; 15.8; 16.7; 16.8 Step six, the preparation of amlodipine:

Add 290 kg of methylamine solution to the reaction kettle.59 kg of phthaloyl amlodipine was added with stirring.Stirring at a temperature of 25 ° C for more than 20 hours,Cool down to 20 ° C, filter, wash the filter residue with drinking water until the pH of the effluent is ≤10,Rinse the filter residue with purified water and drain it.Dry at 60 ° C until moisture ≤ 1.5%,Cooling to normal temperature, discharging, amlodipine, yield 91.6%, purity 99.0%; The 25 kg benzene sulfonic acid, 175 kg purified water added in the dissolving besylate, stirring to dissolve add 1 kg of activated carbon, in the 30 °C stirring under the conditions of the decoloring, filtering, to obtain the sulfonic acid solution, the 40 kg of amlodipine, 250 kg of purified water are added to a reaction kettle stirring, under stirring, to maintain the reaction [...] 30 °C, instillment benzene sulfonic acid solution, canada finishes, in 30 °C conditions for the continuation of stirring, filtering, purifying the water washing until the effluent pH ≥ 3, in 75 °C under drying conditions, until the drying weightlessness ≤ 3.5% discharge, to obtain crude amlodipine besylate, yield 101.0%, purity 99.1%;

References:

CN108456160,2018,A Location in patent:Paragraph 0006; 0014; 0015; 0027-0030

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