Potassium Hydroxide → 1-Chloro-6-fluoro-2-aminonaphthalene

HRID 1270769ノート

反応式

HRID 1270769 の反応式
C(OC(=O)[NH:5][C:6]1[CH:15]=[CH:14][C:13]2[C:8](=[CH:9][CH:10]=[C:11]([F:16])[CH:12]=2)[C:7]=1[Cl:17])C.[OH-].[K+]>C(O)C>[Cl:17][C:7]1[C:8]2[C:13](=[CH:12][C:11]([F:16])=[CH:10][CH:9]=2)[CH:14]=[CH:15][C:6]=1[NH2:5]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 68805760N-(1-chloro-6-fluoro-2-naphthyl)carbamic acid ethyl ester

生成物 1

HCID 184514831-Chloro-6-fluoro-2-aminonaphthalene

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of N-(1-chloro-6-fluoro-2-naphthyl)carbamic acid ethyl ester (600 mg, 2.24 mmol) and KOH (1.51 g, 26.9 mmol) in ethanol (20 mL) is heated to reflux temperature under N2 atmosphere for 12 hours. After cooling, the reaction mixture is concentrated by rotary evaporator. The residual oil is purified by flash chromatography on silica gel (3:1 hexanes/EtOAc) to give 1-chloro-6-fluoro-2-aminonaphthalene as a brown solid.

後処理

  1. temperatureis heated
  2. temperatureto reflux temperature under N2 atmosphere for 12 hours
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture is concentrated by rotary evaporator
  5. customThe residual oil is purified by flash chromatography on silica gel (3:1 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-99f366b8e9874aa299d46b023460aedf
出典データセット
uspto-grants-2007_04
特許番号
US07202364B2

反応ノート

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