Hydrochloric Acid → 1-(5-amino-2-chlorophenyl)ethanone

HRID 1742006ノート

反応式

HRID 1742006 の反応式
[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[CH:7]=[CH:6][C:5]=1[Cl:13])=[O:3].C(O)C.Cl.C(=O)([O-])[O-].[K+].[K+]>O.[Fe]>[CH3:1][C:2]([C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[CH:6][C:5]=1[Cl:13])=[O:3]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 11430Potassium CarbonateHCID 899961-(2-Chloro-5-nitrophenyl)ethan-1-one

生成物 1

HCID 15019111-(5-amino-2-chlorophenyl)ethanone

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒2 回

実験手順

5 g of solid 2-chloro-5-nitroacetophenone (see J. Am. Chem. Soc. 76, 5482 (1952)) are introduced in portions and with stirring at 65° C. to a mixture of 5.6 g of iron powder, 40 ml of ethanol, 9 ml of water and 1 ml of concentrated hydrochloric acid. Stirring of the reaction mixture is continued for 1 hour at 70° C. The mixture is allowed to cool to room temperature and then diluted with 300 ml of water, and a pH of 9 is established by adding 2N potassium carbonate solution. The mixture is filtered with suction through Celite, and the residue is washed with 200 ml of ethyl acetate. The filtrate is transferred to a separating funnel, and the aqueous phase is discarded. The organic phase is washed with saturated sodium chloride solution, dried over sodium sulfate and concentrated.

後処理

  1. filtrationThe mixture is filtered with suction through Celite
  2. washthe residue is washed with 200 ml of ethyl acetate
  3. customThe filtrate is transferred to a separating funnel
  4. washThe organic phase is washed with saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-feb17e5f2234486982ff99672b9803eb
出典データセット
uspto-grants-1994_08
特許番号
US05336663

反応ノート

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