Hydrochloric Acid → (S)-4-(3-methylpiperazin-1-yl)benzonitrile hydrochloride

HRID 2077934

Reaktionsgleichung

Reaktionsgleichung von HRID 2077934
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[C@@H:11]([CH3:22])[CH2:10]2)=[CH:5][CH:4]=1)#[N:2].[ClH:23]>O1CCOCC1.C(OCC)C>[ClH:23].[CH3:22][C@@H:11]1[NH:12][CH2:13][CH2:14][N:9]([C:6]2[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)[CH2:10]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 58324511(S)-tert-butyl 4-(4-cyanophenyl)-2-methylpiperazine-1-carboxylate

Produkt 1

HCID 66775307(S)-4-(3-methylpiperazin-1-yl)benzonitrile hydrochlorideAusbeute 94 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3283Diethyl EtherLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

(S)-tert-butyl 4-(4-cyanophenyl)-2-methylpiperazine-1-carboxylate (0.404 g, 1.340 mmol) was diluted with 4.0M HCl in dioxane (3 mL) and stirred for 30 min. The thick white precipitate that formed was diluted with ethyl ether (10 mL) and stirred until a fine suspension resulted. The precipitate was filtered under nitrogen and dried in vacuum to afford a white solid (300 mg, 94%). [M+H] calc'd for C12H15N3, 201; found, 201.

Aufarbeitung

  1. customThe thick white precipitate that formed
  2. stirringstirred until a fine suspension
  3. customresulted
  4. filtrationThe precipitate was filtered under nitrogen
  5. customdried in vacuum

Quellen und Nachweise

ORD-Eintrag
ord-54081a6d11d74a4586188d899c4d34bc
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928105B2

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