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Ethanol → 1-(2-Carbethoxy-chromon-5-yloxy)-2-hydroxy-3-m-cresyloxypropane

HRID 1606807
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HRID 1606807 반응식
[C:1]([C:4]1[C:22]([OH:23])=[CH:21][CH:20]=[CH:19][C:5]=1[O:6][CH2:7][CH:8]([OH:18])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[CH:12]=1)(=[O:3])[CH3:2].[O-:24][CH2:25][CH3:26].[Na+].[Na].[CH2:29]([OH:31])[CH3:30]>C(OCC)(=O)C(OCC)=O.CCOCC.O.C(O)(=O)C>[C:25]([C:26]1[O:23][C:22]2[C:4]([C:1](=[O:3])[CH:2]=1)=[C:5]([O:6][CH2:7][CH:8]([OH:18])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([CH3:17])[CH:12]=1)[CH:19]=[CH:20][CH:21]=2)([O:31][CH2:29][CH3:30])=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 702EthanolHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 215447821-(2-Acetyl-3-hydroxyphenoxy)-2-hydroxy-3-m-cresyloxypropane

생성물 1

HCID 681392271-(2-Carbethoxy-chromon-5-yloxy)-2-hydroxy-3-m-cresyloxypropane

시약·촉매·용매 4

HCID 176Acetic Acid
용매
HCID 962Water용매
HCID 3283Diethyl Ether용매
HCID 7268Diethyl Oxalate용매

실험 절차

A solution of 1-(2-acetyl-3-hydroxyphenoxy)-2-hydroxy-3-m-cresyloxypropane (25.3 g) in diethyl oxalate (30 ml) was added to a suspension of sodium ethoxide, prepared from sodium (6.0 g) and ethanol (60 ml), in dry ether (400 ml). The mixture was heated under reflux for 1.5 hours; the brown residue was poured onto ice (200 g) and acidified with a solution of acetic acid (24 ml) in water (160 ml). The ether layer was separated after adding more water (200 ml) and the aqueous layer extracted with ether (3 × 50 ml), adding the extracts to the organic layer. The solvent was then removed and the residue dissolved in absolute ethanol (200 ml) to which hydrochloric acid (10 drops) was added. The solution was heated under reflux for 30 minutes and the solvent removed to give a viscous brown oil, which solidified on standing. The oily crystals were filtered off and after recrystallization from aqueous ethanol gave 1-(2-carbethoxy-chromon-5-yloxy)-2 -hydroxy-3-m-cresyloxypropane (8.2 g) as a white solid, m.p. 72°-74°.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. additionthe brown residue was poured onto ice (200 g)
  4. customThe ether layer was separated
  5. additionafter adding more water (200 ml)
  6. extractionthe aqueous layer extracted with ether (3 × 50 ml)
  7. additionadding the extracts to the organic layer
  8. customThe solvent was then removed
  9. dissolutionthe residue dissolved in absolute ethanol (200 ml) to which hydrochloric acid (10 drops)
  10. additionwas added
  11. temperatureThe solution was heated
  12. temperatureunder reflux for 30 minutes
  13. customthe solvent removed
  14. customto give a viscous brown oil, which
  15. filtrationThe oily crystals were filtered off
  16. customafter recrystallization from aqueous ethanol

출처 및 근거

ORD 기록
ord-3d8e1579c8364a7ea2b5f65196c77704
출처 데이터셋
uspto-grants-1976_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03953604

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