Water → HCID 178503587, Verbindung

HRID 2164534Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2164534
Cl.[CH3:2][CH:3]([CH3:7])[C:4](=[NH:6])[NH2:5].[H-].[Na+].[C:10]([C:12](=[C:17](SC)[S:18][CH3:19])[C:13](OC)=[O:14])#[N:11].O>CN(C)C=O>[CH3:2][CH:3]([C:4]1[NH:6][C:17]([S:18][CH3:19])=[C:12]([C:10]#[N:11])[C:13](=[O:14])[N:5]=1)[CH3:7]

Komponenten

6

Edukt 4

HCID 962WaterHCID 24758Sodium hydrideHCID 319957Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoateHCID 27820532-Methylpropanimidamide hydrochloride

Produkt 1

HCID 178503587HCID 178503587, VerbindungAusbeute 89,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel3×

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A solution of 2-methylpropanimidamide hydrochloride (7.0 g, described in Example 7) in dimethylformamide (15 mL) was added dropwise to a suspension of sodium hydride (3.0 g, 50% in mineral oil, prewashed with hexane) in dimethylformamide (15 mL) and the whole mixture was left at 25° C. for 1 hr. 2-Cyano-3,3-bis(methylthio)-2-propenoic acid, methyl ester (6.5 g) in dimethylformamide (15 mL) was then added dropwise, and the reaction mixture was stirred for an additional 4 hr at 25° C. Water (25 mL) was then added, and acidification with concentrated hydrochloric acid (10 mL) precipitated the product. The precipitate was collected and air dried to give the title compound (6.0 g): mp>260° C.

Aufarbeitung

  1. customacidification with concentrated hydrochloric acid (10 mL) precipitated the product
  2. customThe precipitate was collected
  3. customair dried

Quellen und Nachweise

ORD-Eintrag
ord-76a9c31ad9f24d1c811245ad555a643c
Quelldatensatz
uspto-grants-1985_03
Patentnummer
US04505910

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