Reaktionsgleichung
[CH3:1][C@H:2](NC)[C@H:3](O)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1.S(=O)(=O)([O-])N.[NH4+].[NH2:19][C:20]([NH2:22])=[O:21].[CH3:23]N1C(=O)CCC1>O>[CH3:23][N:19]1[CH:2]([CH3:1])[CH:3]([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[NH:22][C:20]1=[O:21]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 177.5 °C
Versuchsvorschrift
1 mol of an ephedrine, 1.025 mol of ammonium sulfamate, 3 mol of urea and the proton-donating compound were introduced into 200 ml of NMP. The reaction mixture was heated to 175 to 180° C. and stirred at this temperature for 2.5 h. It was then cooled to 130° C. and, at this temperature, water was added dropwise to the reaction mixture. Two phases formed. The lower phase was removed at 95° C. The upper phase was further cooled initially to 65° C. Crystals formed at this temperature. It was cooled further to 10° C. and stirred at this temperature for 1 h. The crystals were filtered off with suction and washed twice with cold water. The solid was dried in vacuo at RT overnight.
Aufarbeitung
- additionwas added dropwise to the reaction mixture
- customTwo phases formed
- customThe lower phase was removed at 95° C
- temperatureThe upper phase was further cooled initially to 65° C
- customCrystals formed at this temperature
- temperatureIt was cooled further to 10° C.
- stirringstirred at this temperature for 1 h
- filtrationThe crystals were filtered off with suction
- washwashed twice with cold water
- customThe solid was dried in vacuo at RT overnight
Quellen und Nachweise
- ORD-Eintrag
- ord-0c674f87262c463884a0803402d2a8e9
- Quelldatensatz
- uspto-grants-2008_04
- Patentnummer
- US07365210B2
Verknüpfte Notizen
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