Water → (5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

HRID 1754728ノート

反応式

HRID 1754728 の反応式
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[N:9]=2)=[CH:4][CH:3]=1.[Br:17]N1C(=O)CCC1=O.O>C(#N)C>[Br:17][C:11]1[CH:12]=[CH:13][C:8]([NH:7][CH2:6][C:5]2[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:9][C:10]=1[Cl:14]

参加物

5

反応物 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 57619237(4-Chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine

生成物 1

HCID 57619309(5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

To (4-chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine (538, 4.00 g, 0.0158 mol) in acetonitrile (66.7 mL, 1.28 mol) under an atmosphere of nitrogen, N-bromosuccinimide (2.81 g, 0.0158 mol) in acetonitrile (20 mL) was added slowly. The reaction was stirred at room temperature overnight, then poured into water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, concentrated and crystallized with ethyl acetate in hexane to give a white solid (539, 2.60 g, 95.3%).

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customcrystallized with ethyl acetate in hexane
  5. customto give a white solid (539, 2.60 g, 95.3%)

出典と根拠

ORDレコード
ord-15f917479d7a4133b04098b042ae33c6
出典データセット
uspto-grants-2015_10
特許番号
US09169250B2

反応ノート

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