Potassium Hydroxide → HCID 18317887、化合物

HRID 217241ノート

反応式

HRID 217241 の反応式
[CH3:1][O:2][C:3]([C:5]1([C:10]([O:12]C)=[O:11])[CH2:9][CH2:8][CH2:7][CH2:6]1)=[O:4].[OH-].[K+]>CO>[CH3:1][O:2][C:3]([C:5]1([C:10]([OH:12])=[O:11])[CH2:9][CH2:8][CH2:7][CH2:6]1)=[O:4]

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 12609605Dimethyl cyclopentane-1,1-dicarboxylate

生成物 1

HCID 18317887HCID 18317887、化合物収率 100.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of cyclopentane-1,1-dicarboxylic acid dimethyl ester (4.0 g, 21.5 mmol) in MeOH (25 mL) is added potassium hydroxide (1.32 g, 23.7 mmol). The mixture is stirred at room temperature for 15 hours and concentrated under reduced pressure. To the obtained residue, aqueous 1M HCl (50 mL) is added and the solution is extracted with AcOEt. The organic layer is washed with H2O, dried over Na2SO4, and concentrated under reduced pressure to give cyclopentane-1,1-dicarboxylic acid methyl ester (3.72 g, quant.); TLC (dichloromethane/MeOH, 10:1) Rf 0.25, 1H NMR (400 MHz, chloroform-d) δ ppm 1.67-1.74 (m, 4H), 2.17-2.25 (m, 4H), 3.75 (s, 3H).

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the obtained residue, aqueous 1M HCl (50 mL) is added
  3. extractionthe solution is extracted with AcOEt
  4. washThe organic layer is washed with H2O
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3e284a0d645a4a53a6c42f4f7e887f0b
出典データセット
uspto-grants-2012_06
特許番号
US08193349B2

反応ノート

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