p-Toluenesulfonic acid → HCID 136045554、化合物

HRID 652795ノート

反応式

HRID 652795 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 136045554HCID 136045554、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0fae368c7edf4e358cee98f4b142cb0f
出典データセット
uspto-grants-1987_06
特許番号
US04673692

反応ノート

読み込み中…