Dimethylamine, hydrochloride → HCID 66878630, 화합물
반응식
Cl.[CH3:2][NH:3][CH3:4].[C:5]([O:9][C:10]([C:12]1[CH:20]=[CH:19][C:15]([C:16](O)=[O:17])=[CH:14][C:13]=1[Cl:21])=[O:11])([CH3:8])([CH3:7])[CH3:6]>C(OCC)(=O)C>[Cl:21][C:13]1[CH:14]=[C:15]([C:16](=[O:17])[N:3]([CH3:4])[CH3:2])[CH:19]=[CH:20][C:12]=1[C:10]([O:9][C:5]([CH3:8])([CH3:7])[CH3:6])=[O:11]참가 물질
4
실험 절차
290 mg of dimethylamine hydrochloride was coupled to 1 g of 4-(tert-butoxycarbonyl)-3-chlorobenzoic acid via Procedure G. The reaction mixture was diluted with ethyl acetate, washed with 0.1 N HCl, 0.1 N NaOH and brine, dried (MgSO4) and evaporated to afford tert-butyl 2-chloro-4-(dimethylcarbamoyl)benzoate. 1.1 g of tert-butyl 2-chloro-4-(dimethylcarbamoyl)benzoate was treated with TFA (4 mL) containing trace amounts of H2O for 2 h. The reaction mixture was evaporated, and then added 0.1 N HCl. The resulting solid was filtered and washed with H2O to yield 2-chloro-4-(dimethylcarbamoyl)benzoic acid. 100 mg of 4-chloro-3-(pyridine-2-yl)aniline was coupled to 2-chloro-4-(dimethylcarbamoyl)benzoic acid via Procedure G. The product was purified on reverse phase HPLC to yield 2-chloro-N1-(4-chloro-3-(pyridin-2-yl)phenyl)-N4,N4-dimethylterephthalamide. MS (Q1) 414.1 (M)+.