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Water → HCID 12769816, 화합물

HRID 26682
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HRID 26682 반응식
C([O:3][C:4](=[O:22])[CH:5]([C:7]1[CH:8]=[CH:9][C:10]2[O:15][CH:14]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:13][C:12](=[O:20])[C:11]=2[CH:21]=1)[CH3:6])C.C(=O)(O)[O-].[Na+].O>C(O)C>[CH3:19][C:16]([CH:14]1[CH2:13][C:12](=[O:20])[C:11]2[CH:21]=[C:7]([CH:5]([CH3:6])[C:4]([OH:22])=[O:3])[CH:8]=[CH:9][C:10]=2[O:15]1)([CH3:17])[CH3:18]
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참가 물질

5

반응물 3

HCID 962WaterHCID 516892Sodium BicarbonateHCID 54545077Ethyl-2-[2,3-dihydro-2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate

생성물 1

HCID 12769816HCID 12769816, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl-2-[2,3-dihydro-2-(1,1-dimethylethyl)-4-oxo-4H-1-benzopyran-6-yl]propionate (6 g) was dissolved in ethanol (200 ml) and heated to reflux with dilute aqueous sodium bicarbonate solution (50 ml) for eight hours. The reaction mixture was poured into water, acidified and extracted with ether. The combined ethereal extracts were washed with water and dried (MgSO4) and concentrated in vacuo affording a mixture of the desired product and starting material which were separated by chromatography on silica gel using dichloromethane/ether mixtures as eluant. The title compound was recrystallised from petroleum ether (bp 40°-60° C.) as a white solid: 1.4 g, mp 117°-8° C.

후처리

  1. temperatureheated
  2. extractionextracted with ether
  3. washThe combined ethereal extracts were washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customaffording

출처 및 근거

ORD 기록
ord-d5f1e652cbee44b0891162314319b189
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04151179

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