N-Iodosuccinimide → 7-Chloro-3-iodoimidazo[1,2-b]pyridazine

HRID 407002ノート

反応式

HRID 407002 の反応式
[I:1]N1C(=O)CCC1=O.[Cl:9][C:10]1[CH:15]=[N:14][N:13]2[CH:16]=[CH:17][N:18]=[C:12]2[CH:11]=1>CN(C)C=O.C(OCC)(=O)C>[Cl:9][C:10]1[CH:15]=[N:14][N:13]2[C:16]([I:1])=[CH:17][N:18]=[C:12]2[CH:11]=1

参加物

5

反応物 2

HCID 120273N-IodosuccinimideHCID 679802597-Chloroimidazo(1,2-b)pyridazine

生成物 1

HCID 679805887-Chloro-3-iodoimidazo[1,2-b]pyridazine収率 77.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

N-Iodosuccinimide (2.17 g, 9.65 mmol) was added to a solution of 7-chloroimidazo[1,2-b]pyridazine (0.988 g, 6.43 mmol) in N,N-dimethylformamide (25 mL). The reaction mixture was stirred at r.t. overnight. The mixture was diluted with ethyl acetate, washed with water and brine. The organic layer was dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexane (gradient: 0-50%) to afford the desired product (1.40 g, 77.9%). LCMS (M+H)+: m/z=279.9/281.9.

後処理

  1. washwashed with water and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by flash chromatography on a silica gel column with ethyl acetate in hexane (gradient: 0-50%)

出典と根拠

ORDレコード
ord-a375889df9424b4bb56a380b9e738cfd
出典データセット
uspto-grants-2014_06
特許番号
US08754114B2

反応ノート

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