Sodium Hydroxide → 3-Benzyl-4-chloroaniline

HRID 1111351ノート

反応式

HRID 1111351 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[Al+3].[Cl-].[Cl-].[NH2:11][C:12]1[CH:13]=[CH:14][C:15]([Cl:26])=[C:16]([CH:25]=1)[C:17]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)=O.[OH-].[Na+]>CCOCC.O>[CH2:17]([C:16]1[CH:25]=[C:12]([CH:13]=[CH:14][C:15]=1[Cl:26])[NH2:11])[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 10489713(5-Amino-2-chlorophenyl)(phenyl)methanoneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 221522153-Benzyl-4-chloroaniline

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

6.8 g of lithium aluminium hydride, followed by 44.4 g of aluminium chloride and then 22 g of 5-amino-2-chlorobenzophenone dissolved in anhydrous ether are added in small amounts, under a nitrogen atmosphere, into 1000 ml of anhydrous ether which is cooled to 0° C. After stirring for 2 hours and under reflux, the excessive reagents are decomposed by very slowly adding 7 ml of 15% caustic soda and, finally, 21 ml of water. After filtering and washing the precipitate with 2×200 ml of ether, the organic phase is washed, dried over Na2SO4 and then evaporated to dryness under vacuum.

後処理

  1. temperatureunder reflux
  2. filtrationAfter filtering
  3. washwashing the precipitate with 2×200 ml of ether
  4. washthe organic phase is washed
  5. dry with materialdried over Na2SO4
  6. customevaporated to dryness under vacuum

出典と根拠

ORDレコード
ord-040147399a444ba18ed3d5cb097da47b
出典データセット
uspto-grants-1990_12
特許番号
US04980349

反応ノート

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