Diethyl Ether → HCID 13560729、化合物

HRID 1285488ノート

反応式

HRID 1285488 の反応式
[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]

参加物

7

反応物 5

HCID 3283Diethyl EtherHCID 6344Dichloromethane2 回HCID 517045Sodium AcetateHCID 117900843-(1-Hydroxyhexyl)phenolHCID 178418287HCID 178418287、化合物

生成物 2

HCID 13560729HCID 13560729、化合物HCID 143491261-(3-Hydroxyphenyl)hexan-1-one

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-377e7a5afada46099193a9b330dbe64b
出典データセット
uspto-grants-1986_01
特許番号
US04567184

反応ノート

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