Bromine → 2-Bromo-6-nitro-4-phenoxy-phenylamine

HRID 1466473ノート

反応式

HRID 1466473 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:7]=[CH:6][C:5]=1[NH2:17])([O-:3])=[O:2].[Br:18]Br.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(Cl)Cl>[Br:18][C:6]1[CH:7]=[C:8]([O:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:9]=[C:4]([N+:1]([O-:3])=[O:2])[C:5]=1[NH2:17]

参加物

5

反応物 3

HCID 24408BromineHCID 24477Sodium ThiosulfateHCID 51737522-Nitro-4-phenoxyaniline

生成物 1

HCID 684774322-Bromo-6-nitro-4-phenoxy-phenylamine収率 92%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

2-Nitro-4-phenoxy-phenylamine (2.3 g, 10 mmol) prepared in Preparation 1 was dissolved in DCM (30 mL), Br2 (720 ul, 35%) was added thereto at 0° C., and the mixture was stirred for 2 h. After completion of the reaction, saturated aqueous sodium thiosulfate solution was added. The resulting mixture was extracted with EtOAc, and dried over MgSO4. The solvent was removed under reduced pressure, and the residue was purified by column chromatography to give the title compound (2.84 g, Yield 92%).

後処理

  1. additionwas added
  2. extractionThe resulting mixture was extracted with EtOAc
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-13d261a1ecb548ee8459bb02cd9ef85c
出典データセット
uspto-grants-2015_04
特許番号
US09000028B2

反応ノート

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