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Isopropanol → 2-Amino-4-(4-amino-3,5-dichlorophenoxy)pyridine

HRID 387824
ノート
印刷プレビュー

反応式

HRID 387824 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.[Cl:17]N1C(=O)CCC1=O.C(O)(C)C>O>[NH2:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[C:13]([Cl:17])[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 31398ChlorosuccinimideHCID 229367984-(4-Amino-3-chlorophenoxy)pyridin-2-ylamine

生成物 1

HCID 229363272-Amino-4-(4-amino-3,5-dichlorophenoxy)pyridine収率 15%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Amino-4-(4-amino-3-chlorophenoxy)pyridine (700 mg), N-chlorosuccinimide (0.44 g) and isopropanol (10 ml) were stirred at 80° C. for 1 hour. 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 (ethyl acetate), to obtain 120 mg of a brown oil.

後処理

  1. customwas returned to room temperature
  2. extractionextraction
  3. additionSilica gel was added to the extract solution
  4. distillationthe solvent was distilled off under reduced pressure
  5. additionThe silica gel was charged into a dry column
  6. custompacked with silica gel, and purification

出典と根拠

ORDレコード
ord-fec1ac269d7447ce81dd340ad3d95fbe
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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このページの内容参加物実験手順後処理出典と根拠反応ノート