Diethyl Malonate → Diethyl 2-cyclohexylmethylmalonate

HRID 1060731ノート

反応式

HRID 1060731 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].[CH:13]1([CH2:19]Br)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>C(O)C>[CH:13]1([CH2:19][CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

参加物

5

反応物 3

HCID 7761Diethyl MalonateHCID 137636Cyclohexane, (bromomethyl)-HCID 5360545Sodium

生成物 1

HCID 599487Diethyl 2-cyclohexylmethylmalonate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
70 °C

実験手順

A solution comprised of sodium (6.9 g, 0.3 mmol) in ethanol (250 mL) was treated sequentially with diethyl malonate (53.127 g, 0.3 mol) and then cyclohexylmethyl bromide (46 mL, 0.33 mol) at ambient temperature. The mixture was heated to 70° C. and stirred for approximately 12 hours. The mixture was cooled and solvent was removed by evaporation. The residue was diluted with ice water and the dilution was extracted with ethyl acetate (4×). The combined extracts were washed with water (4×) and brine, dried (MgSO4) and concentrated to provide diethyl 2-cyclohexylmethylmalonate.

後処理

  1. customat ambient temperature
  2. temperatureThe mixture was cooled
  3. customsolvent was removed by evaporation
  4. additionThe residue was diluted with ice water
  5. extractionthe dilution was extracted with ethyl acetate (4×)
  6. washThe combined extracts were washed with water (4×) and brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-f9599f35ecd5494fa60a52163df24231
出典データセット
uspto-grants-2003_02
特許番号
US06525036B2

反応ノート

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