Dichloromethane → HCID 136393672、化合物

HRID 652786ノート

反応式

HRID 652786 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].Cl.[NH2:25][OH:26].[OH-].[K+].ClCCl>C(O)C>[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:25][OH:26])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 14797Potassium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 1898376(3,5-Di-tert-butyl-4-hydroxyphenyl)(phenyl)methanone

生成物 1

HCID 136393672HCID 136393672、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

12.4 g of 3,5-di-t-butyl-4-hydroxybenzophenone and 3.15 g of hydroxylamine hydrochloride were dissolved in 100 ml of ethanol, and with stirring, a solution of 2.77 g of potassium hydroxide in 20 ml of ethanol was added dropwise at room temperature. The mixture was then refluxed for 24 hours with stirring. After cooling, dichloromethane was added to the reaction mixture. The dichloromethane layer was separated, washed with water, and dried. The solvent was distilled off, and n-hexane was added to the residue. The precipitated crystals were collected by filtration, and recrystallized from ether/n-hexane to give 3,5-di-t-butyl-4-hydroxybenzophenone oxime.

後処理

  1. temperatureThe mixture was then refluxed for 24 hours
  2. stirringwith stirring
  3. temperatureAfter cooling
  4. customThe dichloromethane layer was separated
  5. washwashed with water
  6. customdried
  7. distillationThe solvent was distilled off
  8. additionn-hexane was added to the residue
  9. filtrationThe precipitated crystals were collected by filtration
  10. customrecrystallized from ether/n-hexane

出典と根拠

ORDレコード
ord-5d3b0c9d259d4659b91eea4e916ecb27
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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