反応 #50008

反応方程式

2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one

phosphorus oxychloride

→

3-Chloro-2-(2,4-dichloro-6-fluorobenzothiazol-7-yl)-4,5,6,7-tetrahydro-2H-indazole

反応条件

後処理

1. 1
   温度under reflux
2. 2
   温度After cooling
3. 3
   抽出extracted with ethyl acetate
4. 4
   洗浄the organic phase washed with sodium hydrogen carbonate and water
5. 5
   乾燥It was dried over magnesium sulfate
6. 6
   濃縮concentrated
7. 7
   その他The residue was purified by column chromatography

実験手順

0.2 g 2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one was treated with 2 ml phosphorus oxychloride and the mixture stirred for one hour under reflux. After cooling, it was poured into ice-water, extracted with ethyl acetate and the organic phase washed with sodium hydrogen carbonate and water. It was dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 0.07 g=32% of theory m.p.: 161°-163° C.

出典