Morpholine → HCID 18356993, Verbindung

HRID 427288Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 427288
Br[C:2]1[S:3][C:4]2[C:10]([Br:11])=[CH:9][CH:8]=[C:7]([O:12][CH3:13])[C:5]=2[N:6]=1.[NH:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1>O1CCCC1>[Br:11][C:10]1[C:4]2[S:3][C:2]([N:14]3[CH2:19][CH2:18][O:17][CH2:16][CH2:15]3)=[N:6][C:5]=2[C:7]([O:12][CH3:13])=[CH:8][CH:9]=1

Komponenten

4

Edukt 2

HCID 8083MorpholineHCID 183569942,7-Dibromo-4-methoxybenzo[d]thiazole

Produkt 1

HCID 18356993HCID 18356993, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A suspension of 2,7-dibromo-4-methoxybenzothiazole (1.8 g) and morpholine (10 ml) in tetrahydrofuran (10 ml) was heated at 80° C. for 2 hours. The solvent was removed in vacuo and the residue partitioned between ethyl acetate (100 ml) and water (100 ml). The organic layer was dried over magnesium sulphate (3 g), filtered and the filtrate evaporated in vacuo to yield an off white solid. This was purified by recrystallisation from ethyl acetatelhexane to yield the title compound as a white solid (1.2 g). TLC Rf 0.39 (50% ethyl acetate in hexane).

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customthe residue partitioned between ethyl acetate (100 ml) and water (100 ml)
  3. dry with materialThe organic layer was dried over magnesium sulphate (3 g)
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. customto yield an off white solid
  7. customThis was purified by recrystallisation from ethyl acetatelhexane

Quellen und Nachweise

ORD-Eintrag
ord-7d4636cf4b354785b9610c1928f972ff
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313116B1

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