Methanol → HCID 86751694, compound
Reaction equation
[NH2:1][C@H:2]1[C:6]2([CH2:8][CH2:7]2)[CH2:5][N:4]([C:9]2[N:10]([C@@H:25]3[CH2:27][C@@H:26]3[F:28])[C:11]3[C:16]([C:17](=[O:22])[C:18]=2[C:19]([OH:21])=[O:20])=[CH:15][C:14]([F:23])=[CH:13][C:12]=3[Cl:24])[CH2:3]1.CO>O>[OH2:20].[NH2:1][C@H:2]1[C:6]2([CH2:7][CH2:8]2)[CH2:5][N:4]([C:9]2[N:10]([C@@H:25]3[CH2:27][C@@H:26]3[F:28])[C:11]3[C:16]([C:17](=[O:22])[C:18]=2[C:19]([OH:21])=[O:20])=[CH:15][C:14]([F:23])=[CH:13][C:12]=3[Cl:24])[CH2:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 25 °C
Procedure
Crude crystals of 7-[(7-(S)-amino-5-azaspiro[2.4]heptan-5-yl]-8-chloro-6-fluoro-1-[(1R,2S)-2-fluorocyclopropyl]-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (5 g) were added to 150 ml of an aqueous methanol having a water content of 1% or less to form a slurry. The slurry was stirred at 25° C. for 3 days. The crystals were collected by filtration and dried at room temperature under reduced pressure until it was confirmed that the weight became constant to give 4.5 g of the title compound.
Workup
- customto form a slurry
- filtrationThe crystals were collected by filtration
- customdried at room temperature under reduced pressure until it
Sources & evidence
- ORD record
- ord-78e978725e4c4ba3b92725735e726b8c
- Source dataset
- uspto-grants-1997_12
- Patent number
- US05693814
Reaction notes
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