Citric Acid → HCID 19709706, 화합물

HRID 725818노트

반응식

HRID 725818 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 19709706HCID 19709706, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-1f0f09d018f648e7af270eefeb96ac4a
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05707997

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