Sodium hydride → HCID 19744869, 화합물

HRID 1030728노트

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HRID 1030728 반응식
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[C:4]([O:10][CH3:11])[C:3]=1[C:12](=[O:23])[CH2:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=1.[H-].[Na+].Br[CH2:27][C:28]([O:30][CH3:31])=[O:29]>CN(C)C=O>[CH3:9][O:8][C:6]1[CH:5]=[C:4]([O:10][CH3:11])[C:3]([C:12](=[O:23])[CH2:13][CH2:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=2)=[C:2]([O:1][CH2:27][C:28]([O:30][CH3:31])=[O:29])[CH:7]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 60984Methyl bromoacetateHCID 2700571-(2-Hydroxy-4,6-dimethoxyphenyl)-3-(4-methoxyphenyl)-1-propanone

생성물 1

HCID 19744869HCID 19744869, 화합물수율 87.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

Then, 30 ml of dimethylformamide was added to 5.0 g of 1-(2-hydroxy-4,6-dimethoxyphenyl)-3-(4-methoxyphenyl)-1-propanone and 420 mg of sodium hydride, and the mixture was stirred at 0° C. for 1 hour. Then, 2.6 g of methyl α-bromoacetate was added to the mixture, and the mixture was stirred at 0° C. for 1 hour and at room temperature for 1 hour to effect a reaction. After the reaction, the reaction mixture was extracted with ethyl acetate and filtered, and the solvent was removed from the filtrate by distillation. The obtained residue was subjected to the silica gel chromatography [230-400 mesh silica gel; eluting solvent=n-hexane/ethyl acetate (2/1)] and recrystallized from a mixed solvent of diethyl ether and n-hexane to obtain 5.3 g (yield=87.1%) of 1-(4,6-dimethoxy-2-methoxycarbonylmethoxyphenyl)-3-(4-methoxyphenyl)-1-propanone in the form of a colorless plate.

후처리

  1. stirringthe mixture was stirred at 0° C. for 1 hour and at room temperature for 1 hour
  2. customa reaction
  3. customAfter the reaction
  4. extractionthe reaction mixture was extracted with ethyl acetate
  5. filtrationfiltered
  6. customthe solvent was removed from the filtrate by distillation
  7. customrecrystallized from a mixed solvent of diethyl ether and n-hexane

출처 및 근거

ORD 기록
ord-6fec2c2de37948739d3efb1bb554a5ff
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05106871

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