Triethylamine → 5,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine

HRID 352888

Reaktionsgleichung

Reaktionsgleichung von HRID 352888
Br[CH2:2][C:3]1[N:4]=[CH:5][S:6][C:7]=1[CH2:8]Br.Cl.Cl.[CH3:12][NH:13][NH:14][CH3:15].C(N(CC)CC)C>C(O)C>[CH3:12][N:13]1[CH2:2][C:3]2[N:4]=[CH:5][S:6][C:7]=2[CH2:8][N:14]1[CH3:15]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 93801,2-Dimethylhydrazine dihydrochlorideHCID 108496984,5-Bis(bromomethyl)thiazole

Produkt 1

HCID 184427415,6-Dimethyl-4,5,6,7-tetrahydrothiazolo[4,5-d]pyridazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Under ice cooling, 4,5-bis(bromomethyl)thiazole (600 mg) and 1,2-dimethylhydrazine dihydrochloride (294 mg) were suspended in ethanol (20 ml). Triethylamine (1.23 ml) was added in one portion to the reaction mixture, followed by stirring at room temperature for 30 minutes and then, at 50° C. for 30 minutes. The solvent was distilled off and the residue was purified by chromatography on a silica gel column (5% methanol—methylene chloride), whereby the title compound (90 mg, 24%) was obtained.

Aufarbeitung

  1. waitat 50° C. for 30 minutes
  2. distillationThe solvent was distilled off
  3. customthe residue was purified by chromatography on a silica gel column (5% methanol—methylene chloride), whereby the title compound (90 mg, 24%)
  4. customwas obtained

Quellen und Nachweise

ORD-Eintrag
ord-d27dc1db52c34ccfb27bdf9f7684590e
Quelldatensatz
uspto-grants-2004_06
Patentnummer
US06747023B1

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