Citric Acid → HCID 19709706、化合物

HRID 725818ノート

反応式

HRID 725818 の反応式
[C:1](#[N:3])[CH3:2].[CH3:4][C:5]1([CH2:10][CH2:11][C:12](OC)=[O:13])[O:9][CH2:8][CH2:7][O:6]1.[H-].[Na+].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CN(C=O)C>[CH3:4][C:5]1([CH2:10][CH2:11][C:12](=[O:13])[CH2:2][C:1]#[N:3])[O:9][CH2:8][CH2:7][O:6]1

参加物

6

反応物 4

HCID 311Citric AcidHCID 6342AcetonitrileHCID 24758Sodium hydrideHCID 5600311,3-Dioxolane-2-propanoic acid, 2-methyl-, methyl ester

生成物 1

HCID 19709706HCID 19709706、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

An acetonitrile solution (10 ml) containing 5.0 g of methyl 2-methyl-l,3-dioxolane-2-propionate was added dropwise to 10 ml of a DMF suspension containing 2.3 g of 60% sodium hydride, and stirred at room temperature for 4 hours. The reaction mixture was poured into ice water, acidified with a saturated citric acid solution and extracted with ethyl acetate. The organic layer was washed with water and a saturated saline solution and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2) to provide 3.0 g of 2-methyl-β-oxo-1,3-dioxolane-2-pentanenitrile as oil.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. concentrationa saturated saline solution and concentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: n-hexane:ethyl acetate=3:2)

出典と根拠

ORDレコード
ord-1f0f09d018f648e7af270eefeb96ac4a
出典データセット
uspto-grants-1998_01
特許番号
US05707997

反応ノート

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