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Sodium Bicarbonate → HCID 18612735, Verbindung

HRID 1180558
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1180558
[C:1]([NH:4][C:5]1[CH:29]=[CH:28][CH:27]=[CH:26][C:6]=1[CH2:7][N:8]([S:15]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)(=[O:17])=[O:16])[C:9](=[CH2:14])[C:10]([O:12][CH3:13])=[O:11])(=[O:3])[CH3:2].C(=O)(O)[O-].[Na+]>CO>[C:1]([N:4]1[C:5]2[CH:29]=[CH:28][CH:27]=[CH:26][C:6]=2[CH2:7][N:8]([S:15]([C:18]2[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=2)(=[O:17])=[O:16])[CH:9]([C:10]([O:12][CH3:13])=[O:11])[CH2:14]1)(=[O:3])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 516892Sodium Bicarbonate2×HCID 18613053HCID 18613053, Verbindung

Produkt 1

HCID 18612735HCID 18612735, VerbindungAusbeute 79,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of methyl 2-[(2-acetylamino-benzyl)-(4-methoxybenzenesulfonyl)amino]acrylate (8.40 g, 20.07 mmol) in anhydrous methanol (5 ml) was added anhydrous sodium bicarbonate (2.19 g, 26.09 mmol) and the mixture was stirred at room temperature overnight. Anhydrous sodium bicarbonate (2.2 g) was added and the mixture was stirred for 18 hours, heated to 50° C. for three hours and the solvent removed in vacuo. The residue was dissolved in water and ethyl acetate. The organic layer was separated, washed with saturated sodium chloride and dried with anhydrous sodium sulfate. The solvent was removed in vacuo and the residue dried in vacuo to give 6.64 g of white crystals, m.p. 150-155° C.

Aufarbeitung

  1. stirringthe mixture was stirred for 18 hours
  2. temperatureheated to 50° C. for three hours
  3. customthe solvent removed in vacuo
  4. dissolutionThe residue was dissolved in water
  5. customThe organic layer was separated
  6. washwashed with saturated sodium chloride
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe solvent was removed in vacuo
  9. customthe residue dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-21acd2bac17f42238b98403f49c5fd1b
Quelldatensatz
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07282496B2

Notizen zur Reaktion

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