Sodium Hydroxide → Sodium 4-{4-[4-(3-methanesulfonyl-propoxy)-indol-1-yl]-pyrimidin-2-ylamino}-cyclohexanecarboxylate

HRID 237433

Reaktionsgleichung

[OH-].[Na+:2].C[O:4][C:5]([CH:7]1[CH2:12][CH2:11][CH:10]([NH:13][C:14]2[N:19]=[C:18]([N:20]3[C:28]4[C:23](=[C:24]([O:29][CH2:30][CH2:31][CH2:32][S:33]([CH3:36])(=[O:35])=[O:34])[CH:25]=[CH:26][CH:27]=4)[CH:22]=[CH:21]3)[CH:17]=[CH:16][N:15]=2)[CH2:9][CH2:8]1)=[O:6]>O.CC(O)C>[CH3:36][S:33]([CH2:32][CH2:31][CH2:30][O:29][C:24]1[CH:25]=[CH:26][CH:27]=[C:28]2[C:23]=1[CH:22]=[CH:21][N:20]2[C:18]1[CH:17]=[CH:16][N:15]=[C:14]([NH:13][CH:10]2[CH2:11][CH2:12][CH:7]([C:5]([O-:6])=[O:4])[CH2:8][CH2:9]2)[N:19]=1)(=[O:35])=[O:34].[Na+:2]

Komponenten

Reaktionsbedingungen

Temperatur: 82 °C

Versuchsvorschrift

A 50% (w/w) aqueous solution of NaOH in H2O (198.95 g) was added to 4-{4-[4-(3-Methanesulfonyl-propoxy)-indol-1-yl]-pyrimidin-2-ylamino}-cyclohexanecarboxylic acid methyl ester (830.0 g) in IPA (7.5 L) and the mixture allowed to stir at 82° C. for lh and then stirred overnight at room temperature. The mixture was then filtered, and the solid rinsed with IPA, and dried in vacuo at 60° C. for 3 days to yield sodium 4-{4-[4-(3-methanesulfonyl-propoxy)-indol-1-yl]-pyrimidin-2-ylamino}-cyclohexanecarboxylate (96.9%).

Aufarbeitung

stirringstirred overnight at room temperature
filtrationThe mixture was then filtered
washthe solid rinsed with IPA
customdried in vacuo at 60° C. for 3 days

Quellen und Nachweise

ORD-Eintrag: ord-64d79dcc94514b4b9fe9d4334a9a0312
Quelldatensatz: uspto-grants-2014_02
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08642601B2

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