Potassium Hydroxide → 1,3-Dioxaindane-4-carboxylic acid

HRID 380472

반응식

HRID 380472 반응식
[CH2:1]1[O:11][C:10]2[C:3](=[C:4]([CH:7]=[CH:8][CH:9]=2)[CH:5]=[O:6])[O:2]1.[OH-:12].[K+]>CCO.O.[N+]([O-])([O-])=O.[Ag+]>[CH2:1]1[O:11][C:10]2[C:3](=[C:4]([CH:7]=[CH:8][CH:9]=2)[C:5]([OH:12])=[O:6])[O:2]1

참가 물질

6

반응물 2

HCID 14797Potassium HydroxideHCID 822641,3-Benzodioxole-4-carboxaldehyde

생성물 1

HCID 3048321,3-Dioxaindane-4-carboxylic acid

시약·촉매·용매 3

HCID 24470Silver Nitrate촉매HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

To a solution of 0.85 g (5.66 mmol) of 2,3-methylenedioxybenzaldehyde (Aldrich) in EtOH at 0° C. was added a solution of 2.12 g (12.45 mmol) of AgNO3 in 7.5 mL of H2O. To this was then added a solution of 1.74 g (31.4 mmol) of KOH in 12 mL of H2O. After 2 h, the reaction mixture was filtered and the filter was washed with EtOH. The filtrate was concentrated and the pH was adjusted to pH=2 to 3 with 6N HCl. The title compound precipitated out and was isolated by filtration to give the title compound. 1H NMR (CDCl3) δ6.16 (s, 2H), 6.92 (t, 1H, J=8 Hz), 7.04 (d, 1H, J=8 Hz), 7.48 (d, 1H, J=8 Hz);

후처리

  1. filtrationthe reaction mixture was filtered
  2. washthe filter was washed with EtOH
  3. concentrationThe filtrate was concentrated
  4. customThe title compound precipitated out
  5. customwas isolated by filtration

출처 및 근거

ORD 기록
ord-c5c6588803d6433d82995a3d76f74d55
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06303593B1

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