Water → HCID 49766558、化合物

HRID 447050ノート

反応式

HRID 447050 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[OH:11].[Br:12]Br.O>C(Cl)Cl>[NH2:1][C:2]1[C:7]([Br:12])=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[OH:11]

参加物

5

反応物 3

HCID 962WaterHCID 24408BromineHCID 49847212-Amino-5-Nitrophenol

生成物 1

HCID 49766558HCID 49766558、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To an ice-cold solution of 2-amino-5-nitro phenol (40.0 g, 259.52 mmol) in DCM (1.0 L), was added bromine (13.38 mL, 259.52 mmol) drop wise. The resulting reaction mixture was stirred at room temperature for 45 min. After the completion of the reaction (TLC monitoring), water was added and extracted with EtOAc (3×1.0 L). The combined organics was dried over anhydrous Na2SO4 and concentrated under reduced pressure. The crude (55.0 g, 92%) was carried forward to the next step without further purification.

後処理

  1. customThe resulting reaction mixture
  2. additionwas added
  3. extractionextracted with EtOAc (3×1.0 L)
  4. dry with materialThe combined organics was dried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe crude (55.0 g, 92%) was carried forward to the next step without further purification

出典と根拠

ORDレコード
ord-ccc715c7f9624efbb093031d5b468986
出典データセット
uspto-grants-2013_07
特許番号
US08481544B2

反応ノート

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