1,1-Dimethylhydrazine → HCID 136166736、化合物

HRID 652792ノート

反応式

HRID 652792 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].[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

参加物

5

反応物 3

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

生成物 1

HCID 136166736HCID 136166736、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-54c54bad9082412b9192c9549d67a5bf
出典データセット
uspto-grants-1987_06
特許番号
US04673692

反応ノート

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