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

HRID 1769426

反応式

HRID 1769426 の反応式
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

参加物

6

反応物 3

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

生成物 1

HCID 54136641Methyl 4-(2-methoxyethenyl)benzoate収率 80.3%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fd9f31cfc93d46bd8bad2836b65b2953
出典データセット
uspto-grants-1995_01
特許番号
US05380915

関連ノート

読み込み中…