反応 #171752

反応方程式

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

溶媒

ethanol

反応条件

後処理

1. 1
   その他The whole was sealed
2. 2
   温度cooled to room temperature
3. 3
   濃縮concentrated
4. 4
   workup.ADDITIONThe residue was diluted with water
5. 5
   抽出extracted with ethyl acetate
6. 6
   その他The combined organics were purified by reverse phase HPLC

実験手順

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

出典