Diethyl Malonate → 1,3-Diethyl 2-(1-methylbutyl)propanedioate

HRID 992837

反応式

HRID 992837 の反応式
[Na].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].Br[CH:14]([CH2:16][CH2:17][CH3:18])[CH3:15]>C(O)C>[CH2:11]([O:10][C:2](=[O:9])[CH:3]([CH:14]([CH3:15])[CH2:16][CH2:17][CH3:18])[C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH3:12]

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 78902-BromopentaneHCID 5360545Sodium

生成物 1

HCID 954491,3-Diethyl 2-(1-methylbutyl)propanedioate収率 67.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Sodium metal (5.24 g, 0.23 g atm) was reacted with 25 mL of absolute ethanol. To this solution was added dropwise, with stirring, diethyl malonate (36.0 mL, 0.24 mol). The solution was heated to reflux and 2-bromopentane (29.0 mL, 0.23 mol) was added dropwise. After refluxing overnight, the reaction was cooled and the ethanol removed on a rotovap. The product was washed with water, dried with MgSO4 and fractionally distilled to give 35.7 g of the desired product.

後処理

  1. additionTo this solution was added dropwise
  2. temperatureThe solution was heated
  3. temperatureto reflux
  4. temperatureAfter refluxing overnight
  5. temperaturethe reaction was cooled
  6. customthe ethanol removed on a rotovap
  7. washThe product was washed with water
  8. dry with materialdried with MgSO4
  9. distillationfractionally distilled

出典と根拠

ORDレコード
ord-c161b0f5c00a47508e39a5ff3958dd94
出典データセット
uspto-grants-2002_10
特許番号
US06472227B1

関連ノート

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