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Isopropanol → 2-Amino-3-bromo-4-(4-amino-3-chlorophenoxy)pyridine

HRID 387823
ノート
印刷プレビュー

反応式

HRID 387823 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:16])[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[Br:17]N1C(=O)CCC1=O.C(O)(C)C>O>[NH2:1][C:2]1[C:7]([Br:17])=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:16])[CH:10]=2)[CH:5]=[CH:4][N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 3776IsopropanolHCID 67184N-bromobutanimideHCID 229367984-(4-Amino-3-chlorophenoxy)pyridin-2-ylamine

生成物 1

HCID 229362552-Amino-3-bromo-4-(4-amino-3-chlorophenoxy)pyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Amino-4-(4-amino-3-chlorophenoxy)pyridine (1.0 g), N-bromosuccinimide (0.78 g) and isopropanol (10 ml) were stirred for 15 minutes under reflux. The mixture was returned to room temperature, water was added, and extraction was performed with ethyl acetate. Silica gel was added to the extract solution and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel, and purification was performed by column chromatography (hexane:ethyl acetate=2:1, followed by 1:1, ethyl acetate) to obtain 400 mg of the target substance as a brown oil.

後処理

  1. temperatureunder reflux
  2. customwas returned to room temperature
  3. extractionextraction
  4. additionSilica gel was added to the extract solution
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionThe silica gel was charged into a dry column
  7. custompacked with silica gel, and purification
  8. customto obtain 400 mg of the target substance as a brown oil

出典と根拠

ORDレコード
ord-85e6938aa7914932ad6d6ab47596493b
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08372981B2

反応ノート

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