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1-Hexanol → Hexyl (3-cyano-4,5-dimethoxyphenyl)glyoxylate

HRID 725373
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인쇄 미리보기

반응식

HRID 725373 반응식
Br[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([O:15][CH3:16])[C:8]([O:13][CH3:14])=[C:9]([CH:12]=1)[C:10]#[N:11])=[O:4].[Se](=O)=[O:18].[CH2:20]([OH:26])[CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]>C(Cl)Cl>[C:10]([C:9]1[CH:12]=[C:5]([C:3](=[O:4])[C:2]([O:26][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=[O:18])[CH:6]=[C:7]([O:15][CH3:16])[C:8]=1[O:13][CH3:14])#[N:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81031-HexanolHCID 24007Selenium DioxideHCID 214589615-(Bromoacetyl)-2,3-dimethoxybenzonitrile

생성물 1

HCID 17977685Hexyl (3-cyano-4,5-dimethoxyphenyl)glyoxylate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1.45 g of 5-(bromoacetyl)-2,3-dimethoxybenzonitrile and 1.12 g of selenium dioxide are stirred at 120° for 18 hours in 10 ml of n-hexanol. After cooling to room temperature the mixture is diluted with 20 ml of methylene chloride and filtered. The filtrate is washed with water, dried over sodium sulfate and evaporated. The residue is chromatographed on 70 g of silica gel with hexane/ether (2:1). There is obtained hexyl (3-cyano-4,5-dimethoxyphenyl)glyoxylate as an oil.

후처리

  1. filtrationfiltered
  2. washThe filtrate is washed with water
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customThe residue is chromatographed on 70 g of silica gel with hexane/ether (2:1)

출처 및 근거

ORD 기록
ord-3ce1f1d3add64705a6effaf8033de5d9
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05705703

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