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

HRID 1198228노트

반응식

HRID 1198228 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6404ec34562249b5a16439671422a572
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05280032

반응 노트

불러오는 중…