37441-16-0 → HCID 44128653, Verbindung

HRID 2098303Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2098303
[N:1]([CH2:4][CH2:5][S:6][CH3:7])=[C:2]=[O:3].[N+:8](=[C:10]1[N:14]=[CH:13][N:12]=[C:11]1[C:15]([NH2:17])=[O:16])=[N-:9]>CS(C)=O>[CH3:7][S:6][CH2:5][CH2:4][N:1]1[C:2](=[O:3])[N:14]2[CH:13]=[N:12][C:11]([C:15]([NH2:17])=[O:16])=[C:10]2[N:8]=[N:9]1

Komponenten

4

Versuchsvorschrift

1-Isocyanato-2-methylsulfanyl-ethane (1.09 g, 9.31 mmol) was added drop wise to a suspension of 5-diazoimidazole-4-carboxamide (0.5 g, 3.65 mmol) in dry dimethylsulfoxide (5 mL) at room temperature under nitrogen. The resulting mixture was stirred at room temperature overnight. The reaction was quenched by the addition of ice and the solid product (brown) was removed by filtration, washed with Et2O, and purified using flash chromatography (SiO2) using MeCN:CH2Cl2 (0-100% MeCN) Yield: 52 mg, 26%. 1H NMR (400 MHz, d6-DMSO) δ ppm: 8.87 (1H, s), 7.80 (1H, s), 7.66 (1H, s), 4.48 (2H, t), 2.94 (2H, t).

Aufarbeitung

  1. customThe reaction was quenched by the addition of ice
  2. customthe solid product (brown) was removed by filtration
  3. washwashed with Et2O
  4. custompurified

Quellen und Nachweise

ORD-Eintrag
ord-8be1f7dbadd54db2b4922f226690c6d1
Quelldatensatz
uspto-grants-2013_05
Patentnummer
US08450479B2

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