1,1-Dimethylhydrazine → HCID 136166736, 화합물

HRID 652792노트

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HRID 652792 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].[CH3:24][N:25]([CH3:27])[NH2:26].C1(C)C=CC(S(O)(=O)=O)=CC=1>O>[CH3:24][N:25]([CH3:27])[N:26]=[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)[C:7]1[CH:6]=[C:5]([C:1]([CH3:4])([CH3:3])[CH3:2])[C:18]([OH:19])=[C:17]([C:20]([CH3:23])([CH3:22])[CH3:21])[CH:16]=1

참가 물질

5

반응물 3

HCID 59761,1-DimethylhydrazineHCID 6101p-Toluenesulfonic acidHCID 1898376(3,5-Di-tert-butyl-4-hydroxyphenyl)(phenyl)methanone

생성물 1

HCID 136166736HCID 136166736, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

One gram of 3,5-di-t-butyl-4-hydroxybenzophenone was added to 2 ml of 1,1-dimethylhydrazine, and the mixture was heated at 70° to 75° C. for 8 hours in the presence of 20 mg of p-toluenesulfonic acid in autoclave. After cooling, the reaction mixture was poured into water and extracted with diethyl ether. The ethereal layer was washed with water and dried. The ether was distilled, and the residue was chromatographed on a silica gel column, and recrystallized from diethyl ether to give 3,5-di-t-butyl-4-hydroxybenzophenone dimethylhydrazone as pale yellow needles.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with diethyl ether
  3. washThe ethereal layer was washed with water
  4. customdried
  5. distillationThe ether was distilled
  6. customthe residue was chromatographed on a silica gel column
  7. customrecrystallized from diethyl ether

출처 및 근거

ORD 기록
ord-54c54bad9082412b9192c9549d67a5bf
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673692

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