2,6-Dimethylbenzoyl chloride → HCID 21472157、化合物

HRID 2294798ノート

反応式

HRID 2294798 の反応式
[C:1]1([N:7]2[CH2:11][C:10](=[O:12])[NH:9][C:8]2=[O:13])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:14][C:15]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:16]=1[C:17](Cl)=[O:18]>N1C=CC=CC=1>[CH3:14][C:15]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[C:16]=1[C:17]([N:9]1[C:10](=[O:12])[CH2:11][N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:8]1=[O:13])=[O:18]

参加物

4

反応物 2

HCID 890962,6-Dimethylbenzoyl chlorideHCID 5705761-Phenylimidazolidine-2,4-dione

生成物 1

HCID 21472157HCID 21472157、化合物収率 6.3%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

実験手順

In 30 ml of pyridine, were dissolved 1.1 g (6.25 mmol) of 1-phenyl-imidazolidin-2,4-dione and 1.12 g (6.65 mmol) of 2,6-dimethylbenzoyl chloride to conduct a reaction at 60° C. for 3 hours. After completion of the reaction, pyridine was distilled off under reduced pressure, and the resultant residue was subjected to extraction with ethyl acetate. The organic layer was washed with dilute hydrochloric acid and with saturated saline. The thus-washed organic layer was then dried over anhydrous magnesium sulfate, and the solvent was distilled off. The resultant residue was purified by column chromatography on silica gel (developing solvent: n-hexane/ ethyl acetate) and subjected to crystallization from n-hexane/ethyl acetate to obtain 122 mg (yield: 5.8%) of the title compound.

後処理

  1. customa reaction at 60° C. for 3 hours
  2. distillationwas distilled off under reduced pressure
  3. extractionthe resultant residue was subjected to extraction with ethyl acetate
  4. washThe organic layer was washed with dilute hydrochloric acid and with saturated saline
  5. dry with materialThe thus-washed organic layer was then dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off
  7. customThe resultant residue was purified by column chromatography on silica gel (developing solvent: n-hexane/ ethyl acetate)
  8. customsubjected to crystallization from n-hexane/ethyl acetate

出典と根拠

ORDレコード
ord-9ba5dcc641b54c20b4998568fbfd69ad
出典データセット
uspto-grants-1997_11
特許番号
US05691335

反応ノート

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