Epichlorohydrin → 7-(2,3-Epoxypropoxy)-2,2-dimethyl-4-phenylchroman

HRID 224920

반응식

HRID 224920 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[CH2:7][C:8]([CH3:13])([CH3:12])[O:9]2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:26]([CH:28]1[O:30][CH2:29]1)Cl>CC(C)=O>[O:30]1[CH2:29][CH:28]1[CH2:26][O:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([C:14]3[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=3)[CH2:7][C:8]([CH3:13])([CH3:12])[O:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 7835EpichlorohydrinHCID 11430Potassium CarbonateHCID 205705312,2-Dimethyl-7-hydroxy-4-phenylchroman

생성물 1

HCID 233307567-(2,3-Epoxypropoxy)-2,2-dimethyl-4-phenylchroman수율 95%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 7-hydroxy-2,2-dimethyl-4-phenylchroman (11.8 g, 0.046 mole), anhydrous potassium carbonate (11.7 g, 0.093 mole), epichlorohydrin (50 ml) and dry acetone (50 ml) was stirred and boiled under reflux for 6 hours, then cooled and filtered. The filtrate was evaporated in vacuo and the residual brown oil dissolved in ether, washed with water and dried (magnesium sulphate). Removal of the solvent gave 7-(2,3-epoxypropoxy)-2,2-dimethyl-4-phenylchroman as a pale brown solid (13.56 g, 95%), m.p. 82°-85°, after crystallisation from ethanol.

후처리

  1. temperatureunder reflux for 6 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe filtrate was evaporated in vacuo
  5. dissolutionthe residual brown oil dissolved in ether
  6. washwashed with water
  7. dry with materialdried (magnesium sulphate)
  8. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-fa6fa54be04d46ee86d2338b7d31e054
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234726

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