Diethyl Ether → HCID 13560729, 화합물

HRID 1285488노트

반응식

HRID 1285488 반응식
[OH:1][C:2]1[CH:3]=[C:4]([CH:8]([OH:14])[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[CH:5]=[CH:6][CH:7]=1.[Cr](Cl)([O-])(=O)=O.[NH+:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.[C:26]([O-])(=O)[CH3:27].[Na+].[CH3:31][CH2:32]OCC.[CH2:36](Cl)Cl>>[C:8]([C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][CH:5]=1)[O:1][CH2:36][C:21]1[CH:22]=[CH:23][C:24]2[C:25](=[CH:31][CH:32]=[CH:26][CH:27]=2)[N:20]=1)(=[O:14])[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13].[C:8]([C:4]1[CH:3]=[C:2]([OH:1])[CH:7]=[CH:6][CH:5]=1)(=[O:14])[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

참가 물질

7

반응물 5

HCID 3283Diethyl EtherHCID 6344Dichloromethane2회HCID 517045Sodium AcetateHCID 117900843-(1-Hydroxyhexyl)phenolHCID 178418287HCID 178418287, 화합물

생성물 2

HCID 13560729HCID 13560729, 화합물HCID 143491261-(3-Hydroxyphenyl)hexan-1-one

실험 절차

A solution of 1-(3-hydroxyphenyl)-1-hexanol (3 g) (made in Example 1B) in methylene chloride (200 ml) was added to a well-stirred suspension of pyridinium chlorochromate (5.1 g) and sodium acetate (2.5 g) in methylene-chloride (150 ml). The mixture was stirred at room temperature for two hours. Ether (100 ml) was added, and the brown granular precipitate was removed by filtration. All volatiles were removed from the filtrate, and the residual liquid was purified by chromatography on silical gel using ether as eluent. The desired ketone, 3-hexanoylphenol, was isolated as a clear, colorless oil.

후처리

  1. customthe brown granular precipitate was removed by filtration
  2. customAll volatiles were removed from the filtrate
  3. customthe residual liquid was purified by chromatography on silical gel

출처 및 근거

ORD 기록
ord-377e7a5afada46099193a9b330dbe64b
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567184

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