Potassium Carbonate → HCID 57036075, Verbindung

HRID 2260806

Reaktionsgleichung

Reaktionsgleichung von HRID 2260806
Cl[C:2]1[S:6][N:5]=[C:4]([CH3:7])[N:3]=1.[CH3:8][N:9]1[CH2:14][C@@H:13]2[CH2:15][C@H:10]1[CH2:11][NH:12]2.C(=O)([O-])[O-].[K+].[K+]>O1CCCC1.C(Cl)Cl>[CH3:8][N:9]1[CH2:14][C@@H:13]2[CH2:15][C@H:10]1[CH2:11][N:12]2[C:2]1[S:6][N:5]=[C:4]([CH3:7])[N:3]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 11029795(1S,4S)-2-Methyl-2,5-diazabicyclo[2.2.1]heptaneHCID 129191595-Chloro-3-methyl-1,2,4-thiadiazole

Produkt 1

HCID 57036075HCID 57036075, VerbindungAusbeute 36,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6344DichloromethaneLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

A solution of 1.04 g of 5-chloro-3-methyl-1,2,4-thiadiazole, prepared by the procedure of J. Goerdeler, Chim. Ber., 1957, 90, 182, in 2 ml of tetrahydrofuran is added over one hour to a solution of 0.825 g of (S,S)-2-methyl-2,5-diazabicyclo[2.2.1]heptane and 0.77 g of potassium carbonate in 10 ml of tetrahydrofuran. The reaction mixture is stirred at room temperature overnight, diluted with methylene chloride and the organic layer is washed with water. The methylene chloride solution is dried and concentrated in vacuo to dryness. The residue is purified by chromatography (aluminum oxide, Activity Grade 2.5: 2% methyl alcohol/methylene chloride) to give 0.56 g of the desired product:

Aufarbeitung

  1. washthe organic layer is washed with water
  2. dry with materialThe methylene chloride solution is dried
  3. concentrationconcentrated in vacuo to dryness
  4. customThe residue is purified by chromatography (aluminum oxide, Activity Grade 2.5: 2% methyl alcohol/methylene chloride)

Quellen und Nachweise

ORD-Eintrag
ord-8cf852a12857412ebe9b93cbfd6a1649
Quelldatensatz
uspto-grants-1995_12
Patentnummer
US05478939

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