N-methyl-2-pyrrolidone → Formate

HRID 421357

Reaktionsgleichung

Reaktionsgleichung von HRID 421357
Cl[C:2]1[N:3]([CH2:24][CH:25]([CH3:27])[CH3:26])[C:4]2[C:9]([N:10]=1)=[C:8]([N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[N:7]=[C:6]([C:17]1[CH:18]=[N:19][C:20]([NH2:23])=[N:21][CH:22]=1)[N:5]=2.[CH3:28][C@H:29]1[CH2:34][NH:33][CH2:32][CH2:31][NH:30]1.CN1CCCC1=[O:41]>>[CH:15]([O-:14])=[O:41].[CH2:24]([N:3]1[C:2]([N:33]2[CH2:32][CH2:31][NH:30][C@@H:29]([CH3:28])[CH2:34]2)=[N:10][C:9]2[C:4]1=[N:5][C:6]([C:17]1[CH:18]=[N:19][C:20]([NH2:23])=[N:21][CH:22]=1)=[N:7][C:8]=2[N:11]1[CH2:16][CH2:15][O:14][CH2:13][CH2:12]1)[CH:25]([CH3:27])[CH3:26]

Komponenten

5

Edukt 3

HCID 13387N-methyl-2-pyrrolidoneHCID 27342192-Methylpiperazine, (S)-HCID 593335495-(8-Chloro-9-isobutyl-6-morpholino-9H-purin-2-yl)pyrimidin-2-amine

Produkt 2

HCID 283FormateHCID 593335175-{9-Isobutyl-8-[(3S)-3-methylpiperazin-1-yl]-6-morpholin-4-yl-9H-purin-2-yl}pyrimidin-2-amine

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

N-Methylpyrrolidone (2 ml) was added to 5-(8-chloro-9-isobutyl-6-morpholin-4-yl-9H-purin-2-yl)pyrimidin-2-amine (200 mg, 0.51 mmol) and (2S)-2-methylpiperazine (412 mg, 4.1 mmol) and the resulting mixture was stirred at 120° C. for 4 hours. The reaction mixture was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid) to give a formate of the title compound (192 mg) as a white solid.

Aufarbeitung

  1. customThe reaction mixture was purified by preparative HPLC (column, NOMURA Develosil Combi-RP-5; mobile phase, acetonitrile/water/formic acid)

Quellen und Nachweise

ORD-Eintrag
ord-c91aeb8fb32340fd827ace7a10f56977
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08097622B2

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