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Dimethyl malonate → Dimethyl (4-Fluorobenzyl)Malonate

HRID 1795183
ノート
印刷プレビュー

反応式

HRID 1795183 の反応式
[Na].[C:2]([O:9][CH3:10])(=[O:8])[CH2:3][C:4]([O:6][CH3:7])=[O:5].[F:11][C:12]1[CH:19]=[CH:18][C:15]([CH2:16]Br)=[CH:14][CH:13]=1>CO>[CH3:7][O:6][C:4](=[O:5])[CH:3]([CH2:16][C:15]1[CH:18]=[CH:19][C:12]([F:11])=[CH:13][CH:14]=1)[C:2]([O:9][CH3:10])=[O:8]
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 7943Dimethyl malonateHCID 680214-Fluorobenzyl bromideHCID 5360545Sodium

生成物 1

HCID 2781576Dimethyl (4-Fluorobenzyl)Malonate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of anhydrous methanol (250 mL) is added sodium metal (2.875 g, 0.125 mol) piecewise until the evolution of gas has deceased. Dimethyl malonate (16.5 g, 0.125 mol) is added dropwise and the mixture is stirred for 30 minutes. 4-Fluoro benzyl bromide (23.8 g, 0.126 mol) is added dropwise, and the reaction is refluxed for 2 hour. The majority of the solvent is removed under vacuum, and aqueous HCl is added. The solution is extracted with CHCl3, dried, and the solvent removed in vacuo. Distillation of the crude material under reduced pressure provides the desired compound which is used without further purification.

後処理

  1. temperaturethe reaction is refluxed for 2 hour
  2. customThe majority of the solvent is removed under vacuum, and aqueous HCl
  3. additionis added
  4. extractionThe solution is extracted with CHCl3
  5. customdried
  6. customthe solvent removed in vacuo
  7. distillationDistillation of the crude material under reduced pressure

出典と根拠

ORDレコード
ord-21a53e0fc47143a7a0f6a6701eaaedad
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07026335B2

反応ノート

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