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Pyridine → HCID 73867328, Verbindung

HRID 1607845
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1607845
[CH2:1]([O:3][C:4](=[O:11])[CH2:5][NH:6][CH2:7][CH:8]=[CH:9][CH3:10])[CH3:2].N([CH2:15][CH2:16][CH2:17][C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)=C=O.Cl.[NH2:27][OH:28].C([O:34][CH3:35])(OC)OC.[N:36]1C=CC=CC=1>C1COCC1>[OH:28][N:27]=[C:18]([C:20]1[CH:21]=[CH:22][C:23]([NH:36][C:35]([N:6]([CH2:7][CH:8]=[CH:9][CH3:10])[CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:11])=[O:34])=[CH:24][CH:25]=1)[CH2:17][CH2:16][CH3:15]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 1049PyridineHCID 9005Trimethyl orthoformateHCID 443297Hydroxyamine hydrochlorideHCID 22154871HCID 22154871, VerbindungHCID 53851665HCID 53851665, Verbindung

Produkt 1

HCID 73867328HCID 73867328, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 0.02 mol N-2-butenylglycine ethyl ester, prepared as described by S. B. Hyeon, I. Nagai, H. Iesaka, T. Kajita, and M. Furushimain European patent application No. 181,494, in 40 mL of THF is added dropwise to a solution of 0.02 mol of 4-isocyanatobutyrophenone, prepared as described by E. E. Kilbourn, D. L. Peardon, and J. E. Ware in U.S. Pat.No. 3,931,203, and 5 mL of pyridine in 40 mL of THF, and the reaction mixture is stirred for 3 hours. The solvent is then removed by rotary evaporator. The residue is dispersed in 50 mL of CH3OH, and 0.022 mol of hydroxylamine hydrochloride and 0.06 mol of trimethyl orthoformate are added. The reaction mixture is heated to reflux for 1 hour. The solvent is removed by rotary evaporator to give the product, N-[4-(1-hydroxyiminobutyl)phenyl]-N'-(2-butenyl)-N'-ethoxycarbonylmethylurea.

Aufarbeitung

  1. customprepared
  2. customThe solvent is then removed by rotary evaporator
  3. additionThe residue is dispersed in 50 mL of CH3OH
  4. temperatureThe reaction mixture is heated
  5. temperatureto reflux for 1 hour
  6. customThe solvent is removed by rotary evaporator

Quellen und Nachweise

ORD-Eintrag
ord-3c4e4f9c39b74a5183415a19ca6b8cb6
Quelldatensatz
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04868061

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