Ethanol hydrochloride → 1-Acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline

HRID 1107959Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1107959
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][C:17]([OH:19])=[O:18])[CH2:5]1)(=[O:3])[CH3:2].Cl.[CH3:21][CH2:22]O>CCO>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:14])[CH:9]=[C:10]([CH3:13])[CH:11]=2)[CH:6]([CH2:15][CH2:16][C:17]([O:19][CH2:21][CH3:22])=[O:18])[CH2:5]1)(=[O:3])[CH3:2]

Komponenten

4

Versuchsvorschrift

1-Acetyl-3-(2-carboxyethyl)-4,6-dimethylindoline (3.4 g) was dissolved in EtOH (50 ml) and 10N HCl-EtOH (3.9 ml) was added, which was followed by refluxing for 30 min. EtOH was evaporated under reduced pressure and AcOEt (100 ml) was added. After washing with water, the mixture was dried over anhydrous sodium sulfate. AcOEt was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=50/1-10/1) to give 3.3 g of 1-acetyl-3-(2-ethoxycarbonylethyl)-4,6-dimethylindoline.

Aufarbeitung

  1. temperatureby refluxing for 30 min
  2. customEtOH was evaporated under reduced pressure and AcOEt (100 ml)
  3. additionwas added
  4. washAfter washing with water
  5. dry with materialthe mixture was dried over anhydrous sodium sulfate
  6. customAcOEt was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=50/1-10/1)

Quellen und Nachweise

ORD-Eintrag
ord-fc747cbd39a14944a7ad197886069ec6
Quelldatensatz
uspto-grants-2000_05
Patentnummer
US06063806

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