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Ammonium Acetate → 1-Amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one

HRID 1700702
ノート
印刷プレビュー

反応式

HRID 1700702 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([F:16])=[C:6]([CH:8]2[CH2:13][C:12](=O)[CH2:11][C:10](=[O:15])[CH2:9]2)[CH:7]=1.C([O-])(=O)C.[NH4+:21]>C(O)C>[NH2:21][CH:12]1[CH2:13][CH:8]([C:6]2[CH:7]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[F:16])[CH2:9][C:10](=[O:15])[CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517165Ammonium AcetateHCID 183175245-(5-Chloro-2-fluorophenyl)cyclohexane-1,3-dione

生成物 1

HCID 183173031-Amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one収率 72.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5-(5-chloro-2-fluorophenyl)cyclohexane-1,3-dione (2 g) and ammonium acetate (1.9 g) in ethanol (15 ml) was refluxed for 15 hours. The reaction solution was concentrated under reduced pressure, and to the residue were added water (30 ml) and ethyl acetate (150 ml). The mixture was shaken, and the separated upper layer was washed with water and concentrated under reduced pressure. The residue was washed with ethyl acetate and dried to give 1-amino-5-(5-chloro-2-fluorophenyl)cyclohexan-3-one (1.45 g) as yellow crystals.

後処理

  1. concentrationThe reaction solution was concentrated under reduced pressure
  2. additionto the residue were added water (30 ml) and ethyl acetate (150 ml)
  3. washthe separated upper layer was washed with water
  4. concentrationconcentrated under reduced pressure
  5. washThe residue was washed with ethyl acetate
  6. customdried

出典と根拠

ORDレコード
ord-72ae725777ab457b997cae867f223b74
出典データセット
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06350749B1

反応ノート

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