Hydrochloric Acid → Dihydro-2H-pyran-4,4(3H)-dicarboxylic acid

HRID 1351967

反応式

HRID 1351967 の反応式
[O:1]1[CH2:6][CH2:5][C:4]([C:12]([O:14]CC)=[O:13])([C:7]([O:9]CC)=[O:8])[CH2:3][CH2:2]1.Cl>[OH-].[Na+]>[O:1]1[CH2:2][CH2:3][C:4]([C:7]([OH:9])=[O:8])([C:12]([OH:14])=[O:13])[CH2:5][CH2:6]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 239606Diethyl tetrahydropyran-4,4-dicarboxylate

生成物 1

HCID 219303Dihydro-2H-pyran-4,4(3H)-dicarboxylic acid収率 92%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

Diethyl tetrahydro-2H-pyran-4,4-dicarboxylate (4.04 g, 20 mmol) is suspended in a 30% aqueous sodium hydroxide solution (10 mL), and the mixture is stirred at room temperature for 28 hours. The pH value of the reaction solution is adjusted to pH 1 with conc. hydrochloric acid, and the mixture is separated into water and ethyl acetate. The organic layer is dried over anhydrous sodium sulfate, and the solvent is evaporated. Ethyl acetate (30 mL) is added to the obtained crude product, and the mixture is washed by repulping, and the resulting solid is collected by filtration, and dried to give tetrahydro-4H-pyran-4,4-dicarboxylic acid (3.19 g, 18.3 mmol, 92%).

後処理

  1. customthe mixture is separated into water and ethyl acetate
  2. dry with materialThe organic layer is dried over anhydrous sodium sulfate
  3. customthe solvent is evaporated
  4. additionEthyl acetate (30 mL) is added to the
  5. customobtained crude product
  6. washthe mixture is washed
  7. filtrationthe resulting solid is collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-d471813f08b147ca962e4f7fd8269ef9
出典データセット
uspto-grants-2007_05
特許番号
US07217724B2

関連ノート

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