ChemicalBook CAS DataBase List Ufiprazole

Ufiprazole synthesis

12synthesis methods

Product Name:Ufiprazole
CAS Number:73590-85-9
Molecular formula:C17H19N3O2S
Molecular Weight:329.42

37052-78-1 Synthesis

37052-78-1
644 suppliers
$11.00/25g

86604-75-3 Synthesis

2-Chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride

86604-75-3
569 suppliers
$10.00/1g

73590-85-9
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$30.00/10mg

Yield:73590-85-9 100%

Reaction Conditions:

with tetrabutylammomium bromide;edetate disodium;sodium hydroxide in dichloromethane;water; pH=10;pH-value;

Steps:

1.S1-1.S2; 2.S1-2.S2; 3.S1-3.S2; 1.S1-1.S2

Step S1: 80.0 g (0.36 mol) of 4-methoxy-3,5-dimethyl-2-chloromethylpyridine hydrochloride (Compound I) was added to 480 mL of dichloromethane.0.2 g of disodium edetate was dissolved in 80 mL of water and added to the reaction solution.Step S2: After stirring and dissolving, 64.0 g (0.356 mol) was added.2-mercapto-5-methoxybenzimidazole (formula II),2.0 g (0.006 mol, 2% molar equivalent) of tetrabutylammonium bromide,Sodium hydroxide adjusts the pH to 10,Stir until the reaction is over,Liquid separation,extraction,washing,dry,concentrate,a compound of formula III,Calculated in 100% yield.Sodium hydroxide adjusts the pH to 10,The specific adjustment method is:Adjust the pH value in sections,Fine-tuning with 10% sodium hydroxide in the early stage of the reaction;In the middle of the reaction, it was adjusted by using 15% sodium hydroxide.Let it reach a pH of 8,Add 15% sodium hydroxide every 10 minutes.This kind of benefit is adjusted more fully,Can better observe the effect of the adjustment,Make its PH reach 9;In the later part of the reaction, it was adjusted by using 20% hydrogen peroxide.Make it PH to 10,The way the adjustment is added when it is interrupted,Add sodium hydroxide every 20 minutes;By adjusting the pH value in sections,Thereby making the adjusted pH more precise,More saving on sodium hydroxide,Save the production costs of the enterprise.

References:

CN108409714,2018,A Location in patent:Paragraph 0049-0054; 0063-0067; 0076-0080; 0089-0093

37052-78-1 Synthesis

37052-78-1
644 suppliers
$11.00/25g