N-Iodosuccinimide → 5-Iodo-2-methyl-1H-imidazole-4-carbonitrile

HRID 1487865ノート

反応式

HRID 1487865 の反応式
[CH3:1][C:2]1[NH:3][CH:4]=[C:5]([C:7]#[N:8])[N:6]=1.[I:9]N1C(=O)CCC1=O>C(#N)C>[I:9][C:4]1[NH:3][C:2]([CH3:1])=[N:6][C:5]=1[C:7]#[N:8]

参加物

4

反応物 2

HCID 120273N-IodosuccinimideHCID 178432957HCID 178432957、化合物2 回

生成物 1

HCID 900304155-Iodo-2-methyl-1H-imidazole-4-carbonitrile収率 55%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Into a 25-mL round-bottom flask, was placed a mixture of 2-methyl-1H-imidazole-4-carbonitrile (compound 16.3, 50 mg, 0.47 mmol), N-iodosuccinimide (116 mg, 0.52 mmol) in ACN (5 mL). The resulting solution was heated at reflux overnight, then cooled to room temperature and concentrated under reduced pressure. The residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1/2) to yield 60 mg (55%) of the title compound as a light yellow solid.

後処理

  1. customInto a 25-mL round-bottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureat reflux overnight
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography with ethyl acetate/petroleum ether (1/2)

出典と根拠

ORDレコード
ord-c2e7f8662d6145b2861a6a00ddf5e93d
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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