3-Methyl-2-butanone → HCID 66726288, Verbindung

HRID 1024493

Reaktionsgleichung

Reaktionsgleichung von HRID 1024493
[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=O)=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1.[CH3:14][CH:15]([CH3:19])[C:16](=[O:18])[CH3:17].[OH-].[Na+]>CO>[O:1]1[C:7]2[CH:8]=[CH:9][C:10]([CH:12]=[CH:17][C:16](=[O:18])[CH:15]([CH3:19])[CH3:14])=[CH:11][C:6]=2[O:5][CH2:4][CH2:3][CH2:2]1

Komponenten

5

Edukt 3

HCID 112513-Methyl-2-butanoneHCID 14798Sodium HydroxideHCID 27763883,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde

Produkt 1

HCID 66726288HCID 66726288, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

The MeOH (5 mL) solution of 3,4-dihydro-2H-1,5-benzodioxepine-7-carbaldehyde (445 mg) and 3-methyl-2-butanone (195 mg) was treated with aq. sodium hydroxide (1N, 1 ml) and the mixture was stirred for 24 hours. The reaction was partitioned between 10 ml water and 40 ml ethyl acetate. The organic layer was then sequentially washed with aq. hydrochloric acid (1N, 20 ml), water (20 ml), and Brine (20 ml) and then concentrated under reduced pressure. The residue was purified with flash chromatography on silica (33% ethyl acetate in hexane) to give the desired product as a white crystal.

Aufarbeitung

  1. customThe reaction was partitioned between 10 ml water and 40 ml ethyl acetate
  2. washThe organic layer was then sequentially washed with aq. hydrochloric acid (1N, 20 ml), water (20 ml), and Brine (20 ml)
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified with flash chromatography on silica (33% ethyl acetate in hexane)

Quellen und Nachweise

ORD-Eintrag
ord-92691c7ded8f4b29ac0610f63ab42051
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08722896B2

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