Labeint-A9 synthesis

Yield:33254-88-5 93%

Reaction Conditions:

Stage #1: salicylamidewith triethylamine hydrochloride-aluminum trichloride at 20;
Stage #2: chloroacetyl chloride at 45;Reagent/catalyst;Temperature;

Steps:

1

Salicylamide (10 g, 0.073 mol) was added to a three-necked flask,Ionic liquid (triethylamine hydrochloride - aluminum chloride) 50g, to be stirred evenly,Chloroacetyl chloride (20.43g, 0.18mol) was added dropwise at room temperature. After the addition was completed, the oil bath was used to control the reaction temperatureFor 45 reaction, the reaction 2-3h, TCL monitoring reaction, the reaction is completed, extracted 3-4 times with ethyl acetate,The ethyl acetate layer was dried to give 11.14 g of 5-chloroacetylsalicylamide as a white solid, yield 93%.

References:

CN104513177,2017,B Location in patent:Paragraph 0027; 0031; 0036; 0042; 0043; 0049-0050; 0056-0057