Water → HCID 19972899, Verbindung

HRID 1451927Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1451927
[CH3:1][C:2]1[N:3]=[C:4]2[CH:9]=[CH:8][C:7]([C:10]3([C:17](=[S:20])[NH:18][CH3:19])[CH2:15][CH2:14][CH2:13][CH2:12][C:11]3=[O:16])=[CH:6][N:5]2[CH:21]=1.[BH4-].[Na+].O>CO>[OH:16][CH:11]1[CH2:12][CH2:13][CH2:14][CH2:15][C:10]1([C:7]1[CH:8]=[CH:9][C:4]2[N:5]([CH:21]=[C:2]([CH3:1])[N:3]=2)[CH:6]=1)[C:17](=[S:20])[NH:18][CH3:19]

Komponenten

5

Edukt 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 19972896N-Methyl-1-(2-methylimidazo[1,2-a]pyridin-6-yl)-2-oxocyclohexanecarbothioamide

Produkt 1

HCID 19972899HCID 19972899, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

3.03 g of 1-(2-methylimidazo[1,2-a ]pyridin-6-yl)-N-methyl-2-oxocyclohexanecarbothioamide was suspended in 30 ml of methanol. The obtained suspension was cooled with ice, followed by the addition of 0.15 g of sodium borohydride. The obtained mixture was stirred for one hour, followed by the addition of 50 ml of water. The insoluble matter was recovered by filtration and recrystallized from ethanol and then from acetonitrile to give 1.24 g of the title compound (white powder) as a single diastereomer (yield: 41%).

Aufarbeitung

  1. temperatureThe obtained suspension was cooled with ice
  2. filtrationThe insoluble matter was recovered by filtration
  3. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-808f26e9213b4a4c8a95d523e0ffc932
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05605907

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