Sodium Carbonate → 9-Hydroxy-7-(3-methyl-2-octyl)-2,2,-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[c] [1]benzopyran

HRID 267342

반응식

HRID 267342 반응식
[CH3:1][CH:2]([CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:3]([C:5]1[CH:6]=[C:7]([OH:12])[CH:8]=[C:9]([CH:11]=1)[OH:10])[CH3:4].[CH3:18][C:19]1([CH3:30])[CH2:23][C:22](=O)[CH:21]([C:25](OCC)=[O:26])[CH2:20]1.P(Cl)(Cl)(Cl)=O.C(=O)([O-])[O-].[Na+].[Na+]>C1C=CC=CC=1>[OH:10][C:9]1[C:8]2[C:22]3[CH2:23][C:19]([CH3:30])([CH3:18])[CH2:20][C:21]=3[C:25](=[O:26])[O:12][C:7]=2[CH:6]=[C:5]([CH:3]([CH:2]([CH3:1])[CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH3:4])[CH:11]=1

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 24813Phosphorus oxychlorideHCID 2581765-(3-Methyloctan-2-yl)benzene-1,3-diolHCID 11735559Ethyl 4,4-dimethyl-2-oxocyclopentane-1-carboxylate

생성물 1

HCID 541338539-Hydroxy-7-(3-methyl-2-octyl)-2,2,-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[c] [1]benzopyran

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

to 13.5 g. of 5-(3-methyl-2-octyl)-resorcinol and 10.5 g. of 4,4-dimethyl-2-carboethoxycyclopentanone [Canadian J. of Chem. 47, 1982-1988 (1969)] in 59 ml. of benzene was added 4.3 ml. of phosphorus oxychloride with stirring and refluxing for 6 hours. The red solution was let stand at room temperature for 8 hours, poured into ice and sodium carbonate solution. The colorless mixture was extracted with ether, dried over magnesium sulfate and concentrated. The mixture was extracted with cold pentane and the pentane was discarded. The residue [9-hydroxy-7-(3-methyl-2-octyl)-2,2-dimethyl-4-oxo-1,2,3,4-tetrahydrocyclopenta[ c][1]benzopyran] was obtained as a gummy solid.

후처리

  1. temperaturerefluxing for 6 hours
  2. customat room temperature
  3. customfor 8 hours
  4. extractionThe colorless mixture was extracted with ether
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. extractionThe mixture was extracted with cold pentane

출처 및 근거

ORD 기록
ord-11315d3d7c174797a95fe7c427770b3b
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941782

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