Acetone → 4-[(4-Bromophenoxy)methyl]-2,2,4-trimethyl-1,3-dioxolane

HRID 1909091

反応式

HRID 1909091 の反応式
[Br:1][C:2]1[CH:14]=[CH:13][C:5]([O:6][CH2:7][C:8]([CH3:12])([OH:11])[CH2:9][OH:10])=[CH:4][CH:3]=1.[CH3:15][C:16]([CH3:18])=O.O1CCCC1.C(=O)([O-])[O-].[Na+].[Na+]>O.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH2:7][C:8]2([CH3:12])[CH2:9][O:10][C:16]([CH3:18])([CH3:15])[O:11]2)=[CH:13][CH:14]=1

参加物

7

反応物 4

HCID 180Acetone2 回HCID 8028TetrahydrofuranHCID 10340Sodium CarbonateHCID 71059322HCID 71059322、化合物

生成物 1

HCID 710593314-[(4-Bromophenoxy)methyl]-2,2,4-trimethyl-1,3-dioxolane収率 40.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

3-(4-Bromophenoxy)-2-methylpropane-1,2-diol (261 mg, 1.00 mmol), acetone (77 mg, 1.3 mmol), tetrahydrofuran (5 mL), and a boron trifluoride diethyl ether complex (3 drops) were mixed. The mixture was stirred at room temperature for 67 hours, and acetone (102 mg, 1.76 mmol) was added thereto, followed by stirring for 2 hours. Sodium carbonate, ethyl acetate, and water were added to the reaction mixture to conduct extraction. The organic layer was washed with a saline solution twice. A residue was obtained by concentrating the organic layer under reduced pressure, and the residue was subjected to chromatography refining (methylene chloride) using silica gel, obtaining 121 mg of the objective compound (yield: 40%).

後処理

  1. stirringby stirring for 2 hours
  2. extractionextraction
  3. washThe organic layer was washed with a saline solution twice
  4. customA residue was obtained
  5. concentrationby concentrating the organic layer under reduced pressure

出典と根拠

ORDレコード
ord-771e027b372243a5a31bf786fb682a8a
出典データセット
uspto-grants-2013_12
特許番号
US08598358B2

関連ノート

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