2-Phenylpyridine → 2-(2-Bromophenyl)pyridine

HRID 452355ノート

反応式

HRID 452355 の反応式
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Br:13]Br>C(Cl)(Cl)Cl.[Fe]>[Br:13][C:6]1[CH:5]=[CH:4][CH:3]=[CH:2][C:1]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1

参加物

5

反応物 2

HCID 138872-PhenylpyridineHCID 24408Bromine

生成物 1

HCID 132239292-(2-Bromophenyl)pyridine収率 35.4%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

3 g (19.3 mmol) of 2-phenyl pyridine and 40 mg (0.716 mmol) of iron powder were mixed and stirred. It was cooled to 0° C. and 4.0 g (25 mmol) of bromine was added dropwise with stirring, and watching heat generation, and it was raised to 90° C., and stirred for 10 hours. After the reaction, this reaction mixture was dissolved in chloroform to produce a solution, which was washed with 5% sodium thiosulfate aqueous solution. The chloroform solution was dried with sodium sulfate, and then concentrated. The residue was purified by silica gel column chromatography, and the desired 2-(bromophenyl)pyridine was obtained.

後処理

  1. stirringwith stirring
  2. temperaturewatching heat generation, and it
  3. temperaturewas raised to 90° C.
  4. stirringstirred for 10 hours
  5. customAfter the reaction
  6. customto produce a solution, which
  7. washwas washed with 5% sodium thiosulfate aqueous solution
  8. dry with materialThe chloroform solution was dried with sodium sulfate
  9. concentrationconcentrated
  10. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-7a9e177fe2674b13aa753ee058bd7e03
出典データセット
uspto-grants-2013_07
特許番号
US08492007B2

反応ノート

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