반응 #171752

반응 방정식

guanidine hydrochloride

2-(2-chlorophenyl)-1-(4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-3-(dimethylamino)prop-2-en-1-one

potassium carbonate

→

282

5-(2-chlorophenyl)-4-(4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)pyrimidin-2-amine

용매

ethanol

반응 조건

후처리

1. 1
   기타The whole was sealed
2. 2
   온도cooled to room temperature
3. 3
   농축concentrated
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   추출extracted with ethyl acetate
6. 6
   기타The combined organics were purified by reverse phase HPLC

실험 절차

To a solution of crude 2-(2-chlorophenyl)-1-(4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-3-(dimethylamino)prop-2-en-1-one (ca. 0.22 mmol) in ethanol (2 mL) was added potassium carbonate (87 mg, 0.63 mmol) and then guanidine hydrochloride (40 mg, 0.42 mmol). The whole was sealed and heated at 90° C. for 8 h, cooled to room temperature and concentrated. The residue was diluted with water and extracted with ethyl acetate. The combined organics were purified by reverse phase HPLC to give 282. MS (ESI) 406.2

출처