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

HRID 323401노트

반응식

HRID 323401 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c575280252474660a52bde61ea2b6db1
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06211199B1

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