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

HRID 407103ノート

反応式

HRID 407103 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-90cebed63daa45509746536d3028170d
出典データセット
uspto-grants-2014_06
特許番号
US08754219B2

反応ノート

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