Water → 2,3,6-Trifluoro-1-ethylbenzene

HRID 1638684ノート

反応式

HRID 1638684 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].C1(C)C=CC(S(O[CH2:17][CH2:18][C:19]2[C:24]([F:25])=[CH:23][CH:22]=[C:21]([F:26])[C:20]=2[F:27])(=O)=O)=CC=1.O.[OH-].[Na+]>C(OCC)C>[F:27][C:20]1[C:21]([F:26])=[CH:22][CH:23]=[C:24]([F:25])[C:19]=1[CH2:18][CH3:17]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 156318391-[2-(p-Toluenesulfonyloxy)ethyl]-2,3,6-trifluorobenzeneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 148346762,3,6-Trifluoro-1-ethylbenzene収率 116.9%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

Lithium aluminum hydride (5.6 g) is suspended in dry diethyl ether (70 ml) and thereto is added dropwise with stirring a solution of 1-[2-(p-toluenesulfonyloxy)ethyl]-2,3,6-trifluorobenzene (23.3 g) in dry diethyl ether (170 ml) at below 10° C., and the mixture is stirred at room temperature for one hour. To the reaction mixture are added water (5.6 ml), 10% aqueous sodium hydroxide (10.0 ml) and water (5.6 ml) in this order, and the mixture is stirred at room temperature for 30 minutes. The resulting white precipitates are filtered off, and the filtrate is concentrated under atmospheric pressure to give 2,3,6-trifluoro-1-ethylbenzene (13.2 g), as colorless oil.

後処理

  1. additionis added dropwise
  2. stirringthe mixture is stirred at room temperature for 30 minutes
  3. customThe resulting white precipitates
  4. filtrationare filtered off
  5. concentrationthe filtrate is concentrated under atmospheric pressure

出典と根拠

ORDレコード
ord-89d61bddd5724c8da309180f528d100f
出典データセット
uspto-grants-1989_11
特許番号
US04880806

反応ノート

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