1,4-Dioxane → HCID 20038701, Verbindung

HRID 1393639Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1393639
[S:1]1[CH2:5][CH:4]([C:6]([O-])=[O:7])[N:3]([C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])[CH2:2]1.O1CCOCC1.O.[NH3:23]>O1CCCC1>[C:6]([CH:4]1[CH2:5][S:1][CH2:2][N:3]1[C:9]([O:11][C:12]([CH3:15])([CH3:14])[CH3:13])=[O:10])(=[O:7])[NH2:23]

Komponenten

5

Versuchsvorschrift

3-t-Butyl thiazolidine-3,4-dicarboxylate (2.0 g) was dissolved in tetrahydrofuran (10 ml), and N,N′-carbonyl diimidazole (1.4 g) was added thereto with ice-cooling. The mixture was warmed to room temperature and stirred for 6 hours. 1,4-Dioxane (10 ml) was added thereto, and the mixture was added dropwise to 28% ammonia water (40 ml) cooled on an ice bath. The mixture was warmed to room temperature and stirred for 20 hours. The reaction solution was extracted with ethyl acetate (60 ml). The organic phase was washed with a saturated saline solution and dried over sodium sulfate anhydrous. The product was concentrated under reduced pressure to give t-butyl 4-carbamoylthiazolidine-3-carboxylate (1.6 g, Y.:81%).

Aufarbeitung

  1. temperaturewith ice-cooling
  2. temperaturecooled on an ice bath
  3. temperatureThe mixture was warmed to room temperature
  4. stirringstirred for 20 hours
  5. extractionThe reaction solution was extracted with ethyl acetate (60 ml)
  6. washThe organic phase was washed with a saturated saline solution
  7. dry with materialdried over sodium sulfate anhydrous
  8. concentrationThe product was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-f8213438ade54b82b880066a0d1e47dd
Quelldatensatz
uspto-grants-2008_03
Patentnummer
US07345180B2

Notizen zur Reaktion

Wird geladen…