Trimethylsilyl chlorosulphate → HCID 86710120, Verbindung

HRID 1468298

Reaktionsgleichung

Reaktionsgleichung von HRID 1468298
[CH:1]([C:4]1[N:5]=[C:6]2[CH:11]=[C:10]([C:12]#[N:13])[CH:9]=[CH:8][N:7]2[CH:14]=1)([CH3:3])[CH3:2].Cl[S:16]([O:19][Si](C)(C)C)(=[O:18])=[O:17]>ClC(Cl)C>[C:12]([C:10]1[CH:9]=[CH:8][N:7]2[C:14]([S:16]([OH:19])(=[O:18])=[O:17])=[C:4]([CH:1]([CH3:3])[CH3:2])[N:5]=[C:6]2[CH:11]=1)#[N:13]

Komponenten

4

Edukt 2

HCID 78059Trimethylsilyl chlorosulphateHCID 68011330HCID 68011330, Verbindung

Produkt 1

HCID 86710120HCID 86710120, VerbindungAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 63651,1-DichloroethaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

The 2-isopropylimidazo[1,2-a]pyridine-7-carbonitrile (2.00 g, 10.8 mmol) obtained in step 1 of Example 7 was dissolved in dichloroethane (22 mL). Under ice-cooled condition, trimethylsilyl chlorosulfonate (4.08 g, 21.6 mmol) was added, and the mixture was stirred at 100° C. for hours. The solvent was evaporated under reduced pressure, and the residue was slurried in heptane. The resulting crystals were collected by filteration to give 7-cyano-2-isopropylimidazo[1,2-a]pyridine-3-sulfonic acid (2.71 g, yield 95%).

Aufarbeitung

  1. additionwas added
  2. customThe solvent was evaporated under reduced pressure
  3. customThe resulting crystals were collected by filteration

Quellen und Nachweise

ORD-Eintrag
ord-3fd2335cd79c4316a40c234ab5d9d99a
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09000186B2

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