Benzoyl Peroxide → HCID 22615271、化合物

HRID 842708

反応式

HRID 842708 の反応式
C1C(=O)N([Cl:8])C(=O)C1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH3:36])[N:29]=1>C1C=CC=CC=1>[Cl:27][C:28]1[C:33]([C:34]#[N:35])=[CH:32][CH:31]=[C:30]([CH2:36][Cl:8])[N:29]=1

参加物

5

反応物 3

HCID 7187Benzoyl PeroxideHCID 31398ChlorosuccinimideHCID 5204002-Chloro-6-methylpyridine-3-carbonitrile

生成物 1

HCID 22615271HCID 22615271、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

NCS (1.44 g, 10.8 mmol) and benzoyl peroxide (238 mg, 0.98 mmol) were added to a stirred solution of 2-chloro-3-cyano-6-methyl-pyridine (750 mg, 4.92 mmol) in benzene (35 mL) and the mixture was heated to reflux. After 4 h, the mixture was cooled and filtered. The filtrate was diluted with ethyl acetate and was washed with sodium metabisulfite solution, water and brine, dried (Na2SO4) and evaporated in vacuo. The residue was purified by chromatography on silica (chloroform) to give the title compound:

後処理

  1. temperaturethe mixture was heated to reflux
  2. temperaturethe mixture was cooled
  3. filtrationfiltered
  4. additionThe filtrate was diluted with ethyl acetate
  5. washwas washed with sodium metabisulfite solution, water and brine
  6. dry with materialdried (Na2SO4)
  7. customevaporated in vacuo
  8. customThe residue was purified by chromatography on silica (chloroform)

出典と根拠

ORDレコード
ord-770e2c5221a6477481db72971c6ebf26
出典データセット
uspto-grants-2002_04
特許番号
US06376499B1

関連ノート

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