Acetone → Sodium 5-(1,1-dioxido-1,2-thiazinan-2-yl)-7-[({4-fluoro-2-[(methylamino)carbonyl]benzyl}amino)carbonyl]-1,6-naphthyridin-8-olate

HRID 2252805Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2252805
[OH-].[Na+:2].[O:3]=[S:4]1(=[O:36])[CH2:9][CH2:8][CH2:7][CH2:6][N:5]1[C:10]1[N:19]=[C:18]([C:20]([NH:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=2[C:31]([NH:33][CH3:34])=[O:32])=[O:21])[C:17]([OH:35])=[C:16]2[C:11]=1[CH:12]=[CH:13][CH:14]=[N:15]2.CC(C)=O.C(#N)C>O>[O:36]=[S:4]1(=[O:3])[CH2:9][CH2:8][CH2:7][CH2:6][N:5]1[C:10]1[N:19]=[C:18]([C:20]([NH:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=2[C:31]([NH:33][CH3:34])=[O:32])=[O:21])[C:17]([O-:35])=[C:16]2[C:11]=1[CH:12]=[CH:13][CH:14]=[N:15]2.[Na+:2]

Komponenten

6

Versuchsvorschrift

Sodium hydroxide (150 μL, 0.15 mmol, 1N solution) was added to a cloudy solution of 5-(1,1-dioxido-1,2-thiazinan-2-yl)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-8-hydroxy-1,6-naphthyridine-7-carboxamide (73 mg, 0.15 mmol) in a 2 mL mixture of acetone, acetonitrile and water. The homogeneous bright yellow solution was allowed to stir at room temperature for 30 minutes. The solvent was removed in vacuo and dried overnight on the high vac with gentle heating to give the desired product as a bright yellow solid.

Aufarbeitung

  1. customThe solvent was removed in vacuo
  2. customdried overnight on the high vac
  3. temperaturewith gentle heating

Quellen und Nachweise

ORD-Eintrag
ord-d64a7d43a37143dfacef00793149710a
Quelldatensatz
uspto-grants-2008_01
Patentnummer
US07323460B2

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