Pyridinium chloride → 2-Butyl-6-fluoro-5-hydroxy-1-indanone

HRID 7888

反応式

HRID 7888 の反応式
[CH2:1]([CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][C:9]([F:16])=[C:10]([O:14]C)[CH:11]=2)[C:6]1=[O:17])[CH2:2][CH2:3][CH3:4].Cl.N1C=CC=CC=1>>[CH2:1]([CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][C:9]([F:16])=[C:10]([OH:14])[CH:11]=2)[C:6]1=[O:17])[CH2:2][CH2:3][CH3:4]

参加物

3

反応物 2

HCID 10176127Pyridinium chlorideHCID 119529412-Butyl-6-fluoro-5-methoxy-1-indanone

生成物 1

HCID 219908852-Butyl-6-fluoro-5-hydroxy-1-indanone収率 95.1%

反応条件

温度
200 °C

実験手順

A mixture of 2-butyl-6-fluoro-5-methoxy-1-indanone (2.0 g) and pyridine hydrochloride (15.0 g) was heated in an oil bath at 200° C. for 75 minutes. After cooling to room temperature, the mixture was partitioned between EtOAc (100 mL) and water (75 mL) containing brine (25 mL). The organic phase was washed with brine (50 mL), dried over MgSO4, filtered, and evaporated under vacuum to provide 2-butyl-6-fluoro-5-hydroxy-1-indanone (1.79 g) as a solid.

後処理

  1. temperatureAfter cooling to room temperature
  2. customthe mixture was partitioned between EtOAc (100 mL) and water (75 mL)
  3. additioncontaining brine (25 mL)
  4. washThe organic phase was washed with brine (50 mL)
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-1a97121dbeb748ada83910f7c64b7fb6
出典データセット
uspto-grants-2006_08
特許番号
US07087599B2

関連ノート

読み込み中…