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

HRID 1036077ノート

反応式

HRID 1036077 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 97.2%

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 (28) (944 mg, 4 mmol) in 10 ml DCM was added 1 M BBr3 in DCM (8 ml, 8 mmol). The reaction mixture was stirred at r.t. for 2 h, which turned to a brown solution and back to a 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 865 mg of 29 as a brown solid. Yield: 97.2%, 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-d3ff9ed3cc7a414b8f5f0b91e5459e6e
出典データセット
uspto-grants-2013_10
特許番号
US08546403B2

反応ノート

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