O-Methylhydroxylamine hydrochloride → HCID 87222433, Verbindung

HRID 712275Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 712275
Cl.[CH3:2][O:3][NH2:4].[C:5]([C:8]1[C:16]2[S:15][C:14]([NH:17][C:18](=[O:22])[NH:19][CH2:20][CH3:21])=[N:13][C:12]=2[CH:11]=[C:10]([C:23]2[CH:24]=[N:25][C:26]([N:29]3[CH2:34][CH2:33][C:32]([CH3:40])([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH2:31][CH2:30]3)=[N:27][CH:28]=2)[CH:9]=1)(=O)[CH3:6]>CN(C=O)C>[CH2:20]([NH:19][C:18]([NH:17][C:14]1[S:15][C:16]2[C:8](/[C:5](/[CH3:6])=[N:4]/[O:3][CH3:2])=[CH:9][C:10]([C:23]3[CH:28]=[N:27][C:26]([N:29]4[CH2:30][CH2:31][C:32]([CH3:40])([C:35]([O:37][CH2:38][CH3:39])=[O:36])[CH2:33][CH2:34]4)=[N:25][CH:24]=3)=[CH:11][C:12]=2[N:13]=1)=[O:22])[CH3:21]

Komponenten

4

Edukt 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 86663987Ethyl 1-[5-[7-acetyl-2-(ethylcarbamoylamino)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]-4-methyl-piperidine-4-carboxylate

Produkt 1

HCID 87222433HCID 87222433, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

O-Methyl hydroxylamine hydrochloride (64 mg, 0.784 mmol) was added to ethyl 1-[5-[7-acetyl-2-(ethylcarbamoylamino)-1,3-benzothiazol-5-yl]pyrimidin-2-yl]-4-methyl-piperidine-4-carboxylate (200 mg, 0.39 mmol) in DMF (5 mL). The reaction mixture was heated to 60° C. for 4 h after which time LCMS indicated clean conversion to the desired product. The reaction was diluted with EtOAc, washed with water then brine and the organic layer dried (MgSO4), filtered and the solvent removed in vacuo. The crude product obtained was used in the next step.

Quellen und Nachweise

ORD-Eintrag
ord-11fe1b5aad664f1382a5c5a780db6bbe
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09181234B2

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