Triethylamine → 2-(4-Chloro-2-cyanato-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-ethanone

HRID 11723

Reaktionsgleichung

[Cl:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH2:7][C:8]([N:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=3)[CH2:12][C@H:11]2[CH3:24])=[O:9])=[C:4]([OH:27])[CH:3]=1.[CH2:28]([N:30](CC)CC)C.N#CBr>C(Cl)Cl>[Cl:1][C:2]1[CH:26]=[CH:25][C:5]([O:6][CH2:7][C:8]([N:10]2[CH2:15][CH2:14][N:13]([CH2:16][C:17]3[CH:22]=[CH:21][C:20]([F:23])=[CH:19][CH:18]=3)[CH2:12][C@H:11]2[CH3:24])=[O:9])=[C:4]([O:27][C:28]#[N:30])[CH:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: -5 °C

Versuchsvorschrift

To a solution of 2-(4-chloro-2-hydroxy-phenoxy)-1-[4-(4-fluoro-benzyl)-(2R)-2-methyl-piperazin-1-yl]-ethanone (0.168 g, 0.427 mmol) in methylene chloride (2 mL) was added triethylamine (0.12 mL, 0.86 mmol). The solution was cooled to −5° C. via an acetone/ice bath then cyanogen bromide was added (0.22 mL, 0.66 mmol). The reaction was stirred at −5° C. for 30 minutes then concentrated in vacuo to give the crude title compound which was taken directly on to the next step (0.17 g).

Aufarbeitung

concentrationthen concentrated in vacuo

Quellen und Nachweise

ORD-Eintrag: ord-43200a14bd5d42a5942f72c148bce99b
Quelldatensatz: uspto-grants-2006_08
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US07098212B2

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