반응 #80144

반응 방정식

4-chloromethyl-N-{4-methoxy-7-[(2-methoxy-ethyl)-methyl-amino]-benzothiazol-2-yl}-benzamide

N-(2-methoxyethyl)methylamine

→

4-{[(2-methoxy-ethyl)-methyl-amino]-methyl}-N-{4-methoxy-7-[(2-methoxy-ethyl)-methyl-amino]-benzothiazol-2-yl}-benzamide dihydrochloride

수율 168.0%

반응 조건

후처리

1. 1
   기타was ultrasonicated at room temperature for 30 minutes
2. 2
   농축The reaction mixture was then concentrated it vactio
3. 3
   기타the residue purified by flash chromatography (ethyl acetate)
4. 4
   농축The product-containing fractions were concentrated in vactio
5. 5
   여과The resulting crystals were collected by filtration
6. 6
   세척washed with ether

실험 절차

A mixture of 100 mg (0.24 mmol) 4-chloromethyl-N-{4-methoxy-7-[(2-methoxy-ethyl)-methyl-amino]-benzothiazol-2-yl}-benzamide and 212 mg (2.38 mmol) N-(2-methoxyethyl)methylamine was ultrasonicated at room temperature for 30 minutes. The reaction mixture was then concentrated it vactio and the residue purified by flash chromatography (ethyl acetate). The product-containing fractions were concentrated in vactio and the residue stirred with HCl in ether and ethyl acetate. The resulting crystals were collected by filtration and washed with ether to afford 110 mg (91%) 4-{[(2-methoxy-ethyl)-methyl-amino]-methyl}-N-{4-methoxy-7-[(2-methoxy-ethyl)-methyl-amino]-benzothiazol-2-yl}-benzamide dihydrochloride as a white crystalline solid. ES-MS m/e (%): 473 (M+H+, 100).

출처