Lithium Hydroxide → 2,3-Dihydro-8-methoxy-1,4-benzodioxin-6-carboxylic acid

HRID 637135ノート

反応式

HRID 637135 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=12)[C:6]([O:8]C)=[O:7].[OH-].[Li+]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]2[O:16][CH2:15][CH2:14][O:13][C:12]=12)[C:6]([OH:8])=[O:7]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 18464946Methyl 8-Methoxy-2,3-dihydrobenzo[b][1,4]dioxine-6-carboxylate

生成物 1

HCID 49623162,3-Dihydro-8-methoxy-1,4-benzodioxin-6-carboxylic acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Combine methyl 3-methoxy-4,5-ethylenedioxybenzoate (0.46 g, 2.0 mmol) and tetrahydrofuran (15 mL). Add a 1 M aqueous solution of lithium hydroxide (2.5 mL, 2.5 mmol). Heat to reflux. After 15 hours, cool the reaction, concentrate in vacuo to remove most of the tetrahydrofuran. Cool in a ice bath and acidify with a 1 M aqueous hydrochloric acid solution to give a solid. Collect the solid by filtration and dry to give the title compound.

後処理

  1. temperatureHeat to reflux
  2. temperaturecool
  3. customthe reaction
  4. concentrationconcentrate in vacuo
  5. customto remove most of the tetrahydrofuran
  6. temperatureCool in a ice bath
  7. customto give a solid
  8. customCollect the solid
  9. filtrationby filtration
  10. customdry

出典と根拠

ORDレコード
ord-21a77e9b1a4140b7938a4963cd8cc960
出典データセット
uspto-grants-2001_02
特許番号
US06194406B1

反応ノート

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