反応 #320057

反応方程式

sodium boron hydride

2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-11-oxo-6,11-dihydrodibenz[b,e]oxepine

sodium boron hydride

→

title compound

収率 72.1%

2-(7-Chloro-6-fluoroquinolin-2-yl)methoxy-11-hydroxy-6,11-dihydrodibenz[b,e]oxepine

収率 72.1%

溶媒

methanol

反応条件

後処理

1. 1
   その他obtained in Reference example 34
2. 2
   workup.STIRRINGDuring stirring
3. 3
   その他After completion of the reaction
4. 4
   その他the solvent was removed under reduced pressure, ice water
5. 5
   workup.ADDITIONwas added to the residue
6. 6
   抽出the mixture was extracted with methylene chloride
7. 7
   洗浄Then, the organic layer was washed with water
8. 8
   乾燥dried over anhydrous sodium sulfate
9. 9
   その他the solvent was removed
10. 10
    洗浄The resulting solid was washed with a methylene chloride-hexane mixed solution

実験手順

0.5 g of sodium boron hydride was added to 2.58 g of 2-(7-chloro-6-fluoroquinolin-2-yl)methoxy-11-oxo-6,11-dihydrodibenz[b,e]oxepine obtained in Reference example 34 suspended in 70 ml of methanol and the mixture was stirred at room temperature for 11 hours. During stirring, 0.35 g of sodium boron hydride was added to the mixture twice. After completion of the reaction, the solvent was removed under reduced pressure, ice water was added to the residue and the mixture was extracted with methylene chloride. Then, the organic layer was washed with water and then dried over anhydrous sodium sulfate and the solvent was removed. The resulting solid was washed with a methylene chloride-hexane mixed solution to obtain 1.87 g of the title compound. Mass (CI); m/z=422 (M+ +1)

出典