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Methyl Ethyl Ketone → HCID 21474593, 화합물

HRID 2256352
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HRID 2256352 반응식
[CH3:1][C:2]1([CH3:15])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[C:7](=O)[CH2:6][CH:5]=[CH:4][C:3]1=2.[OH:16][C:17]1[CH:26]=[C:25]([OH:27])[CH:24]=[C:23]([OH:28])[C:18]=1[C:19]([O:21][CH3:22])=[O:20].C(=O)([O-])[O-].[K+].[K+].[CH2:35]([C:37](C)=[O:38])C>>[OH:16][C:17]1[CH:26]=[C:25]([O:27][CH2:35][C:37]([C:6]2[CH:5]=[CH:4][C:3]3[C:2]([CH3:15])([CH3:1])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]=3[CH:7]=2)=[O:38])[CH:24]=[C:23]([OH:28])[C:18]=1[C:19]([O:21][CH3:22])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 76600Methyl 2,4,6-trihydroxybenzoateHCID 86751137HCID 86751137, 화합물

생성물 1

HCID 21474593HCID 21474593, 화합물

실험 절차

3.1 g (10 mmol) of 2-(2'-bromoaceto)-(5,6,7,8-tetrahydro-5,5,8,8-tetramethylnaphthone, 1.8 g (10 mmol) of methyl 2,4,6-trihydroxybenzoate, 1.4 g (10 mmol) of potassium carbonate and 100 ml of methyl ethyl ketone are introduced into a flask. The mixture is heated under reflux for 1 hour and evaporated to dryness. The residue is taken up with water and dichloromethane, and the organic phase is separated, dried over magnesium sulphate and evaporated. The residue obtained is purified by chromatography on a silica column, eluted with a mixture of dichloromethane and hexane (50:50). After evaporation of the solvents, 2.2 g (53%) of the expected product of melting point 169°-170° C. are collected.

후처리

  1. temperatureThe mixture is heated
  2. temperatureunder reflux for 1 hour
  3. customevaporated to dryness
  4. customthe organic phase is separated
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue obtained
  8. customis purified by chromatography on a silica column
  9. washeluted with a mixture of dichloromethane and hexane (50:50)
  10. customAfter evaporation of the solvents, 2.2 g (53%) of the expected product of melting point 169°-170° C.
  11. customare collected

출처 및 근거

ORD 기록
ord-e03fe56085384b3080410b0f969b8328
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05654331

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