Dimethylformamide → Ethyl 2-[4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenoxy]acetate

HRID 747584노트

반응식

HRID 747584 반응식
CN(C)C=O.[OH:6][CH:7]([C:13]1[C:18]([CH3:19])=[CH:17][C:16]([OH:20])=[C:15]([CH3:21])[CH:14]=1)[CH:8]([O:11][CH3:12])[O:9][CH3:10].C(=O)([O-])[O-].[K+].[K+].Cl[CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31]>C(OCC)(=O)C>[OH:6][CH:7]([C:13]1[C:18]([CH3:19])=[CH:17][C:16]([O:20][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])=[C:15]([CH3:21])[CH:14]=1)[CH:8]([O:9][CH3:10])[O:11][CH3:12]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 117758724-(1-Hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenol

생성물 1

HCID 10470761Ethyl 2-[4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenoxy]acetate수율 77.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To N,N-dimethylformamide (81 g) were added 4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenol (20.0 g), potassium carbonate (15.8 g) and ethyl chloroacetate (12.4 g) at room temperature with stirring. The mixture was stirred at room temperature for an hour, and then stirred at 71° C. for 2 hours. The reaction mixture was diluted with ethyl acetate, washed with water and brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and a mixture of ethyl acetate and hexane was added to the residue. The precipitated crystals were collected by filtration to give ethyl 2-[4-(1-hydroxy-2,2-dimethoxyethyl)-2,5-dimethylphenoxy]acetate (21.3 g).

후처리

  1. stirringThe mixture was stirred at room temperature for an hour
  2. stirringstirred at 71° C. for 2 hours
  3. washwashed with water and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationThe organic layer was concentrated under reduced pressure
  6. additiona mixture of ethyl acetate and hexane
  7. additionwas added to the residue
  8. filtrationThe precipitated crystals were collected by filtration

출처 및 근거

ORD 기록
ord-5ca95b95d2f34c89965372610487f8d8
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07396954B2

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