p-Toluenesulfonic acid → HCID 136045554, 화합물

HRID 652795노트

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HRID 652795 반응식
[C:1]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])[C:18]=1[OH:19])[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=O)([CH3:4])([CH3:3])[CH3:2].[NH2:24][NH:25][C:26]([NH2:28])=[S:27].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[C:1]([C:5]1[CH:6]=[C:7]([CH:16]=[C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])[C:18]=1[OH:19])[C:8](=[N:24][NH:25][C:26]([NH2:28])=[S:27])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 1898376(3,5-Di-tert-butyl-4-hydroxyphenyl)(phenyl)methanoneHCID 2723789Thiosemicarbazide

생성물 1

HCID 136045554HCID 136045554, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

6.2 g of 3,5-di-t-butyl-4-hydroxybenzophenone and 2.2 g of thiosemicarbazide were dissolved in 20 ml of toluene, and 0.4 g of p-toluenesulfonic acid was added. The solution was refluxed for 16 hours while removing water. After the reaction, dilute hydrochloric acid was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and dried, and the solvent was distilled off under reduced pressure. The residue was chromatographed on a silica gel column, and recrystallized from dichloromethane/n-hexane to give 3,5-di-t-butyl-4-hydroxybenzophenone thiosemicarbazone.

후처리

  1. temperatureThe solution was refluxed for 16 hours
  2. customwhile removing water
  3. customAfter the reaction, dilute hydrochloric acid
  4. additionwas added
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. customdried
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was chromatographed on a silica gel column
  10. customrecrystallized from dichloromethane/n-hexane

출처 및 근거

ORD 기록
ord-0fae368c7edf4e358cee98f4b142cb0f
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673692

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