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

HRID 1158783

反応式

HRID 1158783 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e8f123f0f43c459098a2e50796ba7a4a
出典データセット
uspto-grants-2010_10
特許番号
US07812019B2

関連ノート

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