Hydrochloric Acid → HCID 68907622, Verbindung

HRID 1510347Notizen

Reaktionsgleichung

[NH2:1][C:2]1([CH3:30])[C:6]2([CH2:8][CH2:7]2)[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:28])[C:14]([C:25]([OH:27])=[O:26])=[CH:15][N:16]3[C@@H:21]3[CH2:23][C@@H:22]3[F:24])=[CH:11][C:10]=2[F:29])[CH2:3]1.[ClH:31].C(O)(C)C>CO>[ClH:31].[NH2:1][C:2]1([CH3:30])[C:6]2([CH2:7][CH2:8]2)[CH2:5][N:4]([C:9]2[C:18]([O:19][CH3:20])=[C:17]3[C:12]([C:13](=[O:28])[C:14]([C:25]([OH:27])=[O:26])=[CH:15][N:16]3[C@@H:21]3[CH2:23][C@@H:22]3[F:24])=[CH:11][C:10]=2[F:29])[CH2:3]1

Komponenten

Reaktionsbedingungen

Temperatur: 50 °C

Versuchsvorschrift

7-[7-amino-7-methyl-5-azaspiro[2.4]heptan-5-yl]-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-8-methoxy-1,4-dihydro-4-oxoquinoline-3-carboxylic acid in which configuration of the amino group in the substituent at position 7 is the same as the one produced in Example 9 (18.07 g, 39.4 mmol) was suspended in methanol (54 mL), and 1N hydrochloric acid (43.4 mL, 43.4 mmol) was added to the suspension at room temperature. Isopropyl alcohol (180 mL) was then added, and the mixture was stirred in a water bath at 50° C. for some time until precipitated gummy material thoroughly turned to crystal. After allowing to stand at room temperature for 1 hour, the crystals were collected by filtration, and washed with a small amount of isopropyl alcohol (twice). The crystals were then dried under reduced pressure to obtain the title compound 12.91 g (27.2 mmol, 69%) as a yellow powder.

Aufarbeitung

customuntil precipitated gummy material
filtrationthe crystals were collected by filtration
washwashed with a small amount of isopropyl alcohol (twice)
customThe crystals were then dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-35a1ccec0aaf47c3855a95ed3574e80e
Quelldatensatz: uspto-grants-2012_07
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08211910B2

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