Prilocaine synthesis
- Product Name:Prilocaine
- CAS Number:721-50-6
- Molecular formula:C13H20N2O
- Molecular Weight:220.31
107-10-8
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$10.00/20mg
7623-09-8
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$38.50/25g
95-53-4
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$10.00/1g
721-50-6
443 suppliers
$12.00/1mg
Yield:721-50-6 97%
Reaction Conditions:
Stage #1:2-chloropropionyl chloride;o-toluidine with potassium carbonate in acetone at 0 - 30; for 5 h;
Stage #2:propylamine in acetone at 70; for 14 h;
Steps:
1
(A) 300 g of o-toluidine, 390 g of K2C03 was added to a 2000 ml three-necked flask (refiner)Three bottles of acetone added 1500ml, 0 ° C ice bath slowly dropping α-chloro propionyl chloride 340ml, control the bottle temperature does not exceed 30 ° C, 3h drop to complete. Dichloride: petroleum ether = 1: 3, adding 2 drops of glacial acetic acid) to detect the disappearance of raw materials after the treatment, the reactants into the big beaker Add water 2000ml precipitation of solid, filtered 4 times washed with water, each with 100ml water washing, drying, solid 60 ° C blast drying, the intermediate 490 grams, the yield was 88.4%. (B) Weigh 120 mg of propylamine cocaine, 80 g of K2C03, and 400 ml of acetone, and the mixture of propylamine,Potassium added to the three bottles, and then add acetone, and then dropping n-propylamine l0ml, warming to 70 ° C, reflux reaction 14h, TLC monitoring reaction is complete. (Ethyl acetate: petroleum ether = 1: 3). The filtrate was dried under reduced pressure and dried. After extraction with ethyl acetate, the filtrate was dried with anhydrous sodium sulfate, the organic layer was frozen and the crystals were crystallized , And the crystals were filtered at room temperature by 25 ° (3 vacuum drying to obtain about 129 g of prilocaine, the yield was 97.0%
References:
Jinan Chenghui Shuangda Chemical Co., Ltd;Wang, Ting Jian;Guo, inventor Yang;Yang, Yanjun;Li, Yue Dong;Liu, Zhiwen CN104529812, 2016, B Location in patent:Paragraph 0051; 0052
107-10-8
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$10.00/20mg
19281-31-3
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$45.00/10mg
721-50-6
443 suppliers
$12.00/1mg