2-(Tert-butoxy)ethan-1-ol → 1-(3-Chlorophenyl)-2-(2-tertbutoxyethoxy)ethanol

HRID 1198228ノート

反応式

HRID 1198228 の反応式
CC(C)([O-])C.[K+].[C:7]([O:11][CH2:12][CH2:13][OH:14])([CH3:10])([CH3:9])[CH3:8].[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]2[CH2:24][O:23]2)[CH:19]=[CH:20][CH:21]=1>C(OCC)(=O)C>[Cl:15][C:16]1[CH:17]=[C:18]([CH:22]([OH:23])[CH2:24][O:14][CH2:13][CH2:12][O:11][C:7]([CH3:10])([CH3:9])[CH3:8])[CH:19]=[CH:20][CH:21]=1

参加物

5

反応物 3

HCID 242322-(Tert-butoxy)ethan-1-olHCID 1556132-(3-Chlorophenyl)oxiraneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 538355021-(3-Chlorophenyl)-2-(2-tertbutoxyethoxy)ethanol

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

5.1 g of potassium tert-butoxide was added to 105 ml of ethylene glycol mono-tert-butyl ether. The mixture was heated to 80° C. Thereto was dropwise added 35.0 g of 2-(3-chlorophenyl)oxirane over 1 hour. The mixture was stirred for 2 hours at the same temperature. The reaction mixture was added to a mixture of 100 ml of ice water and 100 ml of ethyl acetate. The organic layer was separated, washed with a saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue thus obtained was subjected to further distillation under reduced pressure to obtain 37.7 g of colorless oily 1-(3-chlorophenyl)-2-(2-tert-butoxyethoxy)ethanol having a boiling point of 140°-146° C./0.9 mmHg.

後処理

  1. customover 1 hour
  2. customThe organic layer was separated
  3. washwashed with a saturated aqueous sodium chloride solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed by distillation under reduced pressure
  6. customThe residue thus obtained
  7. distillationwas subjected to further distillation under reduced pressure

出典と根拠

ORDレコード
ord-6404ec34562249b5a16439671422a572
出典データセット
uspto-grants-1994_01
特許番号
US05280032

反応ノート

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