ChemicalBook CAS DataBase List 2-Amino-6-chlorobenzoic acid

2-Amino-6-chlorobenzoic acid synthesis

11synthesis methods

Product Name:2-Amino-6-chlorobenzoic acid
CAS Number:2148-56-3
Molecular formula:C7H6ClNO2
Molecular Weight:171.58

A, in the reaction vessel being provided with agitator, thermometer, reflux condenser, Dropping funnel, add cerium chloride 0.16mol, 4-hydroxy 3-methoxybenzene ethanol solution 0.19mol, Klorvess Liquid 400-500ml, control mixing speed and exist 160-190rpm, rising solution temperature, to 60-65°C, is slowly added to 2-chloro-6-nitrobenzoyl acid solution 0.13mol, sulfurous acid Hydrogen potassium solution 200ml, raises mixing speed to 260-310rpm, back flow reaction 5-7h；
B, reduction solution temperature, to 15-19°C, separate out solid, filter, and add diammonium hydrogen citrate solution 150-in filtrate 180ml, concentrating under reduced pressure, separate out solid, filter, dehydrant is dehydrated, brine, and pyridine solution washs, ethyl acetate solution Middle recrystallization, obtains crystal 2-amino-6-chlorobenzoic acid (C7H6ClNO2).

5344-49-0 Synthesis

5344-49-0
147 suppliers
$10.00/5g

2148-56-3
359 suppliers
$5.00/10g

Yield:2148-56-3 90%

Reaction Conditions:

with potassium bisulfite;cerium(III) chloride;potassium chloride;2-methoxy-phenol in ethanol at 65; for 8 h;Time;

Steps:

6 Example 6
The mass fraction of the potassium bisulfite solution in Example 1 was adjusted, and the remaining preparation conditions were mixed with the raw materialsIn the same manner as in Example 1, the reaction yield was as follows Example 1A, In a reaction vessel equipped with a stirrer, a thermometer, a reflux condenser, and a dropping funnel, cerium chloride0.16mol, mass fraction 23% 4-hydroxy-3-methoxybenzene ethanol solution 0.19mol, mass fraction of 28% potassium chloride solution 500ml, control the stirring speed 190rpm, raising the solution temperature to 65 , slow Adding 0.13mol of 2-chloro-6-nitrobenzoic acid solution, adding 200ml of 41% potassium bisulfite solution, increasing the stirring speed to 310rpm and refluxing for 5h;B, reduce the solution temperature to 19 ° C, precipitation of solid, filtration, the filtrate was added to the mass fraction of 49% hydrogen dihydrogen citrateAmmonium hydroxide solution, 180ml, concentrated under reduced pressure, precipitated solid, filtered, dehydrated calcium oxide dehydration agent, sodium bromide solution, washed 72% pyridine solution, mass fraction of 78% ethyl acetate solution recrystallization,

References:

Chengdu East Power Technology Co., Ltd. Al;Chu, Donghong CN105801443, 2016, A Location in patent:Paragraph 0023; 0024; 0025; 0026; 0027; 0047; 0048-0050

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616224-61-4 Synthesis