反応 #348742

反応方程式

2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one

sodium boron hydride

→

2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol

溶媒

methanol

methanol

反応条件

後処理

1. 1
   温度cooling over a period of 5 minutes
2. 2
   その他the mixture was reacted at room temperature for 30 minutes
3. 3
   温度refluxed for 15 minutes
4. 4
   workup.DISTILLATIONwas distilled off
5. 5
   温度After cooling, to the mixture
6. 6
   workup.ADDITIONwas added water
7. 7
   抽出the mixture was extracted with chloroform
8. 8
   洗浄The extract was washed with water
9. 9
   乾燥dried over anhydrous sodium sulfate

実験手順

To the mixture of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one obtained in Example 40 and 10 ml of methanol was gradually added 0.2 g of sodium boron hydride with ice-cooling over a period of 5 minutes and the mixture was reacted at room temperature for 30 minutes and refluxed for 15 minutes. After the completion of the reaction, methanol was distilled off. After cooling, to the mixture was added water and the mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and freed of the solvent to obtain 0.5 g of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol as colorless crystals having a melting point of 130°-132° C.

出典