2,6-Dimethylbenzoyl chloride → HCID 21472157, 화합물

HRID 2294798노트

반응식

HRID 2294798 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 21472157HCID 21472157, 화합물수율 6.3%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9ba5dcc641b54c20b4998568fbfd69ad
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05691335

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