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Carbon Dioxide → 7-BROMO-2,3-DIMETHYL-1-BENZOFURAN

HRID 1107863
ノート
印刷プレビュー

反応式

HRID 1107863 の反応式
S(=O)(=O)(O)O.C(=O)=O.[Br:9][C:10]1[CH:21]=[CH:20][CH:19]=[CH:18][C:11]=1[O:12][CH:13]([CH3:17])[C:14](=O)[CH3:15]>CC(C)=O>[CH3:17][C:13]1[O:12][C:11]2[C:10]([Br:9])=[CH:21][CH:20]=[CH:19][C:18]=2[C:14]=1[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 280Carbon DioxideHCID 1118Sulfuric AcidHCID 15381110HCID 15381110、化合物

生成物 1

HCID 110962627-BROMO-2,3-DIMETHYL-1-BENZOFURAN収率 91.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

25 ml of concentrated sulphuric acid are introduced into a 100 ml three-necked flask equipped with a thermometer and a 10 ml dropping funnel and cooling is carried out to between -15 and 0° C. with a bath of solid carbon dioxide in acetone. 3-(2-Bromophenoxy)-2-butanone (5 g, 20.6 mmol) is added dropwise and stirring is continued for 5 min. The mixture is poured onto crushed ice and then extraction is carried out with ethyl acetate (3×80 ml). The organic phases are combined, dried over magnesium sulphate and concentrated. The residue is purified by silica column chromatography (elution solvent: cyclohexane). 4.24 g (Yield: 91%) of 2,3-dimethyl-7-bromobenzofuran are obtained--M.p.: 33° C.

後処理

  1. customequipped with a thermometer
  2. temperaturecooling
  3. additionThe mixture is poured
  4. customonto crushed ice
  5. extractionextraction
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated
  8. customThe residue is purified by silica column chromatography (elution solvent: cyclohexane)

出典と根拠

ORDレコード
ord-3967f8d9b6504b879c696d25a1cd0ce8
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06063810

反応ノート

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