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

HRID 838895

反応式

HRID 838895 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 7-hydroxy-2,2-dimethyl-4-phenylchroman (11.8g, .046 mole), anhydrous potassium carbonate (11.7g, 0.093 mole), epichlorohydrin (50ml) and dry acetone (50ml) 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 (13.56g, 95%), m.p. 82°-85°, after crystallization from ethanol.

後処理

  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

出典と根拠

ORDレコード
ord-635f87242d28449a9321f53824cbd9d3
出典データセット
uspto-grants-1978_06
特許番号
US04093631

関連ノート

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