Carbon Dioxide → 13-Methyltetradecanoic Acid

HRID 1872806노트

반응식

HRID 1872806 반응식
[Mg].Br[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH:14]([CH3:16])[CH3:15].[C:17](=[O:19])=[O:18].Cl>O1CCCC1.C(OCC)(=O)C>[CH3:15][CH:14]([CH3:16])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][C:17]([OH:19])=[O:18]

참가 물질

7

반응물 4

HCID 280Carbon DioxideHCID 313Hydrochloric AcidHCID 5462224MagnesiumHCID 110657331-Bromo-12-methyltridecane

생성물 1

HCID 15101413-Methyltetradecanoic Acid수율 57.5%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

Magnesium (1.5 g) was added to a solution of 1-bromo-12-methyltridecane (15.0 g) in tetrahydrofuran (200 ml). The mixture was refluxed for 10 minutes under nitrogen atmosphere and stirred for 1 hour at room temperature. A solid of carbon dioxide (50 g) was added to the mixture. To the mixture was added a mixture of 1% hydrochloric acid (300 ml) and ethyl acetate (150 ml). The organic layer was washed with water, dried over magnesium sulfate and evaporated. The residue was chromatographed on a silica gel column eluting with chloroform to give 13-methyltetradecanoic acid as an oil (7.54 g).

후처리

  1. temperatureThe mixture was refluxed for 10 minutes under nitrogen atmosphere
  2. additionTo the mixture was added
  3. washThe organic layer was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated
  6. customThe residue was chromatographed on a silica gel column
  7. washeluting with chloroform

출처 및 근거

ORD 기록
ord-92bc3fe3dd68485fabfdb41338a743c4
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06110933

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