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

HRID 1107863
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HRID 1107863 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 280Carbon DioxideHCID 1118Sulfuric AcidHCID 15381110HCID 15381110, 화합물

생성물 1

HCID 110962627-BROMO-2,3-DIMETHYL-1-BENZOFURAN수율 91.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3967f8d9b6504b879c696d25a1cd0ce8
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06063810

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