Hydrochloric Acid → HCID 69299496, Verbindung

HRID 2196500Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2196500
[C:1]([C:3]1[S:7][CH:6]=[C:5]([N:8](C(OC(C)(C)C)=O)[NH:9]C(OC(C)(C)C)=O)[CH:4]=1)#[N:2].[ClH:24].O1CCOCC1>CC(O)C>[ClH:24].[NH:8]([C:5]1[CH:4]=[C:3]([C:1]#[N:2])[S:7][CH:6]=1)[NH2:9]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59843278Di-tert-butyl 1-(5-cyanothiophen-3-yl)hydrazine-1,2-dicarboxylate

Produkt 1

HCID 69299496HCID 69299496, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

To a stirring solution of compound 12 (1.38 g, 4.07 mmol) in 2-propanol (10 mL) was added 4M HCl in dioxane (10 mL, 40.0 mmol). The reaction heated to 80 degrees for 1 hour turning into a dark brown solution. The mixture was evaporated to dryness and the resulting the brown solid suspended and sonicated in diethyl ether. The suspension was filtered to afford compound 13 (0.701 g, 97%) as a brown solid. LRMS (ESI): calc. 139.0; found 140.1 (MH)+.

Aufarbeitung

  1. temperatureThe reaction heated to 80 degrees for 1 hour
  2. customThe mixture was evaporated to dryness
  3. customsonicated in diethyl ether
  4. filtrationThe suspension was filtered

Quellen und Nachweise

ORD-Eintrag
ord-7e624a66ce7e4c598f259738cf1ddbb4
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08338437B2

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