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

HRID 380472

反応式

HRID 380472 の反応式
[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

参加物

6

反応物 2

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

生成物 1

HCID 3048321,3-Dioxaindane-4-carboxylic acid

試薬・触媒・溶媒 3

HCID 24470Silver Nitrate触媒HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

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);

後処理

  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

出典と根拠

ORDレコード
ord-c5c6588803d6433d82995a3d76f74d55
出典データセット
uspto-grants-2001_10
特許番号
US06303593B1

関連ノート

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