Dichloromethane → HCID 136393672, 화합물

HRID 652786노트

반응식

HRID 652786 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].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]

참가 물질

6

반응물 4

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

생성물 1

HCID 136393672HCID 136393672, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5d3b0c9d259d4659b91eea4e916ecb27
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673692

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