Tetrahydrofuran → HCID 53871027, Verbindung

HRID 1419709Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1419709
C[Mg]Cl.O1CCC[CH2:5]1.Cl[C:10]1[S:11][C:12]2[CH:18]=[C:17]([F:19])[CH:16]=[C:15]([Cl:20])[C:13]=2[N:14]=1.[Cl-].[NH4+]>C(OCC)C.Cl[Ni](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[Cl:20][C:15]1[C:13]2[N:14]=[C:10]([CH3:5])[S:11][C:12]=2[CH:18]=[C:17]([F:19])[CH:16]=1

Komponenten

7

Edukt 4

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 534405702,4-Dichloro-6-fluoro-1,3-benzothiazoleHCID 178418332HCID 178418332, Verbindung

Produkt 1

HCID 53871027HCID 53871027, VerbindungAusbeute 49,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418751HCID 178418751, VerbindungKatalysatorHCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

67 ml of a solution of methyl magnesium chloride in tetrahydrofuran (3M; 0.2 mol) were added dropwise to a solution of 22 g (0.1 mol) of 2,4-dichloro-6-fluorobenzothiazole and 3.3 g (5 mmol) of dichlorobis(triphenylphosphine)nickel in 100 ml of diethyl ether. After stirring had been carried out for 2 hours, the mixture was poured onto saturated aqueous ammonium chloride solution. The desired product was extracted with diethyl ether, after which the combined organic phases were washed with water, dried over magnesium sulfate and finally evaporated down. 10 g of the desired product were obtained by crystallization from petroleum ether.

Aufarbeitung

  1. extractionThe desired product was extracted with diethyl ether
  2. washafter which the combined organic phases were washed with water
  3. dry with materialdried over magnesium sulfate
  4. customfinally evaporated down

Quellen und Nachweise

ORD-Eintrag
ord-82e7a942b1ef455fb8614a838e5d0e60
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05888940

Notizen zur Reaktion

Wird geladen…