Methyl 4-Formylbenzoate → Methyl 4-(2-methoxyethenyl)benzoate

HRID 1769426

반응식

HRID 1769426 반응식
C([Li])CCC.[Br-].[CH3:7][O:8][CH2:9][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH:29]([C:31]1[CH:40]=[CH:39][C:34]([C:35]([O:37][CH3:38])=[O:36])=[CH:33][CH:32]=1)=O>CCCCCC.O1CCCC1>[CH3:7][O:8][CH:9]=[CH:29][C:31]1[CH:40]=[CH:39][C:34]([C:35]([O:37][CH3:38])=[O:36])=[CH:33][CH:32]=1

참가 물질

6

반응물 3

HCID 15294Methyl 4-FormylbenzoateHCID 2773654(Methoxymethyl)triphenylphosphonium bromideHCID 178418339Butyllithium

생성물 1

HCID 54136641Methyl 4-(2-methoxyethenyl)benzoate수율 80.3%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

In an atmosphere of argon, a solution containing butyllithium dissolved in hexane was added to a solution containing 120 g of methoxymethyltriphenylphosphonium bromide dissolved in tetrahydrofuran (THF), and the mixture was stirred for one hour at room temperature. A solution containing 50 g of methyl 4-formylbenzoate dissolved in THF was added thereto, and stirring was continued for two hours. The reaction solution was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography to obtain 47 g of methyl 4-(2-methoxyethenyl)benzoate (45).

후처리

  1. additionwas added to a solution
  2. additionwas added
  3. stirringstirring
  4. waitwas continued for two hours
  5. washThe reaction solution was washed with water
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-fd9f31cfc93d46bd8bad2836b65b2953
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05380915

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