Chlorosuccinimide → 6-Bromo-5-chloropyridin-2-amine

HRID 1521933ノート

反応式

HRID 1521933 の反応式
[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][CH:3]=1.[Cl:9]N1C(=O)CCC1=O>C(#N)C>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[Cl:9]

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 3008092-Amino-6-bromopyridine

生成物 1

HCID 534011936-Bromo-5-chloropyridin-2-amine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

To a solution of 6-bromopyridin-2-amine (1 g, 5.78 mmol) in acetonitrile (10 mL) was added N-chlorosuccinimide (0.849 g, 6.36 mmol) and the mixture was heated at 80° C. for 12 hours. The mixture was filtered through diatomaceous earth and concentrated and the residue was dissolved in ethyl acetate and washed with water and brine. Drying over anhydrous sodium sulfate, filtration, concentration and purification by column chromatography (silica gel, 30% ethyl acetate in hexane) afforded the title compound. LCMS: 209.1 (M+2)+.

後処理

  1. filtrationThe mixture was filtered through diatomaceous earth
  2. concentrationconcentrated
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washwashed with water and brine
  5. dry with materialDrying over anhydrous sodium sulfate, filtration, concentration and purification by column chromatography (silica gel, 30% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-2d5fb1cc5f4c4a46be44fd6fc7fba095
出典データセット
uspto-grants-2015_07
特許番号
US09073922B2

反応ノート

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