Sodium Iodide → HCID 21995698、化合物

HRID 1978737ノート

反応式

HRID 1978737 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([CH3:9])[C:3]=1[CH3:10].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].Cl[CH2:20][CH2:21][O:22][CH2:23][CH2:24][CH3:25]>CN(C=O)C.O>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:20][CH2:21][O:22][CH2:23][CH2:24][CH3:25])=[C:4]([CH3:9])[C:3]=1[CH3:10]

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 1235061-(2-Chloroethoxy)propaneHCID 139746564-Bromo-2,3-dimethylphenol

生成物 1

HCID 21995698HCID 21995698、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

In DMF (82 ml) was dissolved 4-bromo-2,3-dimethylphenol (8.2 g). To the mixture were added potassium carbonate (7.3 g) and sodium iodide (6.1 g) and then was added dropwise 2-chloroethylpropylether (6.2 ml), and the mixture was stirred at 90 for 10 hours and cooled to room temperature. The reaction mixture was added to water, and the mixture was extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated, and the residue was purified with silica gel column chromatography (hexane/ethyl acetate=12/1) to give 4-bromo-2,3-dimethyl-1-(2-propoxyethoxy)benzene (7.5 g).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried with magnesium sulfate
  4. customUnder reduced pressure, the solvent was evaporated
  5. customthe residue was purified with silica gel column chromatography (hexane/ethyl acetate=12/1)

出典と根拠

ORDレコード
ord-01afa9d67e644610905bb7bfc7e5f6a4
出典データセット
uspto-grants-2001_05
特許番号
US06235771B1

反応ノート

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