StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Sodium Hydroxide → 2,4-Dichloro-7-(6,6-dimethyl-3,5,6,7-tetrahydropyrrolo-[2,1-c][1,2,4]thiadiazol-3-ylidenamino)-6-fluorobenzothiazole

HRID 21729
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 21729
[Cl:1][C:2]1[S:3][C:4]2[C:10]([N:11]=[C:12]=[S:13])=[C:9]([F:14])[CH:8]=[C:7]([Cl:15])[C:5]=2[N:6]=1.Cl.[NH2:17][C:18]1[NH:19][CH2:20][C:21]([CH3:24])([CH3:23])[CH:22]=1.[OH-].[Na+].BrBr>ClCCl.O>[Cl:1][C:2]1[S:3][C:4]2[C:10]([N:11]=[C:12]3[S:13][N:17]=[C:18]4[CH2:22][C:21]([CH3:24])([CH3:23])[CH2:20][N:19]34)=[C:9]([F:14])[CH:8]=[C:7]([Cl:15])[C:5]=2[N:6]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 14798Sodium HydroxideHCID 24408BromineHCID 199334612-Amino-4,4-dimethylpyrroline hydrochlorideHCID 199334642,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole

Produkt 1

HCID 539682062,4-Dichloro-7-(6,6-dimethyl-3,5,6,7-tetrahydropyrrolo-[2,1-c][1,2,4]thiadiazol-3-ylidenamino)-6-fluorobenzothiazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel3×

Reaktionsbedingungen

Temperatur
2 °C

Versuchsvorschrift

A solution of 2 g 2,4-dichloro-6-fluoro-7-isothiocyanatobenzothiazole in 10 ml dichloromethane was added, dropwise, at 0° C., to a suspension of 1.1 g 2-amino-4,4-dimethylpyrroline hydrochloride in 20 ml dichloromethane. A solution of 0.3 g sodium hydroxide and 6 ml water was added, dropwise, at 2° C. to this mixture which was stirred for 3 hours, whereby the temperature rose to 20° C. The mixture was cooled to -10° C. and a solution of 1 g bromine in 10 ml dichloromethane was added, dropwise, slowly and the mixture stirred for I hour whereby the temperature rose to 10° C. The solution was washed with water and with dilute caustic soda, dried over magnesium sulfate and concentrated. The residue was recrystallised from diisopropyl ether. Yield: 1.5 g=53% of theory m.p.: 134°-136° C.

Aufarbeitung

  1. customrose to 20° C
  2. temperatureThe mixture was cooled to -10° C.
  3. stirringdropwise, slowly and the mixture stirred for I hour whereby the temperature
  4. customrose to 10° C
  5. washThe solution was washed with water and with dilute caustic soda
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated
  8. customThe residue was recrystallised from diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-d804bd441201440e948ae6abc9e51e2d
Quelldatensatz
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05424443

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion