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Sodium Bicarbonate → HCID 178449933, Verbindung

HRID 1906696
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1906696
[C:1]([CH:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])(=O)[CH2:2][CH2:3][CH3:4].[Cl-].[CH2:25]([O:27][NH3+:28])[CH3:26].C(=O)(O)[O-].[Na+]>CO>[CH2:25]([O:27][NH:28][C:1](=[C:6]1[C:11](=[O:12])[CH2:10][CH:9]([CH:13]2[CH2:19][CH2:18][O:17][CH:16]([CH:20]([CH3:22])[CH3:21])[O:15][CH2:14]2)[CH2:8][C:7]1=[O:23])[CH2:2][CH2:3][CH3:4])[CH3:26]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 516892Sodium BicarbonateHCID 13473084HCID 13473084, VerbindungHCID 19001768HCID 19001768, Verbindung

Produkt 1

HCID 178449933HCID 178449933, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

6.5 parts by weight of 2-butyryl-5-(2-isopropyl-1,3-dioxepan-5-yl)-cyclohexane-1,3-dione, 2.1 parts by weight of ethoxyammonium chloride and 1.8 parts by weight of sodium bicarbonate in 80 parts by volume of methanol are stirred for 16 hours at room temperature. The solvent is distilled off under reduced pressure, the residue is stirred with 50 parts by volume of water and 50 parts by volume of dichloromethane, the organic phase is separated off, the aqueous phase is extracted once with 50 parts by volume of dichloromethane, the combined organic phases are dried over sodium sulfate, and the solvent is distilled off under reduced pressure. 6.2 parts by weight of 2-(1-ethoxyamino-n-butylidene)-5-(2-isopropyl1,3-dioxepan-5-yl)-cyclohexane-1,3-dione are obtained as an oil (active ingredient No. 1).

Aufarbeitung

  1. distillationThe solvent is distilled off under reduced pressure
  2. customthe organic phase is separated off
  3. extractionthe aqueous phase is extracted once with 50 parts by volume of dichloromethane
  4. dry with materialthe combined organic phases are dried over sodium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-efad078866f64c24ab5a3d1d248f69ab
Quelldatensatz
uspto-grants-1987_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04654073

Notizen zur Reaktion

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