Potassium Carbonate → 2-[2-(3-Tert-butyl-phenoxy)-ethyl]-[1,3]dioxane

HRID 1158783

반응식

HRID 1158783 반응식
[C:1]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].Br[CH2:13][CH2:14][CH:15]1[O:20][CH2:19][CH2:18][CH2:17][O:16]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[C:1]([C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][CH:10]=1)[O:11][CH2:13][CH2:14][CH:15]1[O:20][CH2:19][CH2:18][CH2:17][O:16]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 11450Phenol, 3-(1,1-dimethylethyl)-HCID 5206561,3-Dioxane, 2-(2-bromoethyl)-

생성물 1

HCID 595485522-[2-(3-Tert-butyl-phenoxy)-ethyl]-[1,3]dioxane수율 112.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

3-tert-butyl-phenol (1.50 g, 10 mmol), 2-(2-bromo-ethyl)-[1,3]dioxane (1.38 g, 10 mmol) and potassium carbonate (2.15 g, 11 mmol) in 20 ml acetonitrile was heated to reflux for 16 hours. After cooling, the solvent was removed under reduced pressure and the residue partitioned between diethyl ether and water. The isolated organic layer was washed with water, dried with magnesium sulfate, filtered and the solvent removed under reduced pressure to give 2.97 g of crude 2-[2-(3-tert-butyl-phenoxy)-ethyl]-[1,3]dioxane, which was used without further purification.

후처리

  1. temperatureto reflux for 16 hours
  2. temperatureAfter cooling
  3. customthe solvent was removed under reduced pressure
  4. customthe residue partitioned between diethyl ether and water
  5. washThe isolated organic layer was washed with water
  6. dry with materialdried with magnesium sulfate
  7. filtrationfiltered
  8. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-e8f123f0f43c459098a2e50796ba7a4a
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812019B2

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