Boron tribromide → 2-Amino-5-bromo-4-chlorophenol

HRID 530781ノート

反応式

HRID 530781 の反応式
[Br:1][C:2]1[CH:8]=[C:7]([O:9]C)[C:5]([NH2:6])=[CH:4][C:3]=1[Cl:11].B(Br)(Br)Br>C(Cl)Cl>[NH2:6][C:5]1[CH:4]=[C:3]([Cl:11])[C:2]([Br:1])=[CH:8][C:7]=1[OH:9]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 229976674-Bromo-5-chloro-2-methoxyaniline

生成物 1

HCID 584871002-Amino-5-bromo-4-chlorophenol収率 101.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 4-bromo-3-chloro-6-methoxyaniline (52) (5 g, 21.1 mmol) in 50 ml DCM was added 1 M BBr3 in DCM (43 ml, 43 mmol) at 0° C. The reaction mixture was stirred at r.t. for 3 h, which turned to a light brown solution and back to a light brown suspension. After quenched with aq. sodium bicarbonate solution, the mixture was extracted with EA. The org. phase was washed with brine, dried over sodium sulfate, concentrated to dryness to give 4.746 g 53 as light brown solid. Yield: 100%, purity>95%.

後処理

  1. customAfter quenched with aq. sodium bicarbonate solution
  2. extractionthe mixture was extracted with EA
  3. washphase was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-417b84f831ab4cca88b4f3931d1264e9
出典データセット
uspto-grants-2016_05
特許番号
US09353099B2

反応ノート

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