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

HRID 1256786ノート

反応式

HRID 1256786 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-7c0633e9578541c5a392e68ceda18369
出典データセット
uspto-grants-2013_06
特許番号
US08461169B2

反応ノート

読み込み中…