Azane;hydrate → HCID 67236507, compound

HRID 2356385Notes

Reaction equation

HRID 2356385 reaction equation
FC(F)(F)C(O)=O.[NH2:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:28][C@@H:27]3[C@@H:22]([CH2:23][CH2:24][CH2:25][NH:26]3)[CH2:21]2)[C:16]([O:29][CH:30]([F:32])[F:31])=[C:15]2[C:10]=1[C:11](=[O:39])[C:12]([C:36]([OH:38])=[O:37])=[CH:13][N:14]2[CH:33]1[CH2:35][CH2:34]1.O.N>>[NH2:8][C:9]1[C:18]([F:19])=[C:17]([N:20]2[CH2:28][C@@H:27]3[C@@H:22]([CH2:23][CH2:24][CH2:25][NH:26]3)[CH2:21]2)[C:16]([O:29][CH:30]([F:31])[F:32])=[C:15]2[C:10]=1[C:11](=[O:39])[C:12]([C:36]([OH:38])=[O:37])=[CH:13][N:14]2[CH:33]1[CH2:35][CH2:34]1

Participants

3

Reactant 2

HCID 12896473Azane;hydrateHCID 86615170HCID 86615170, compound

Product 1

HCID 67236507HCID 67236507, compound

Procedure

The preparation comprises neutralizing 5-amino-1-cyclopropyl-8-difluoromethoxyl-7-(cis-2,8-diazabicyclo[4,3,0]nonane-8-yl)-6-fluoro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid trifluoroacetate (target product of embodiment 19, 3.0 g) with ammonia water, refrigerating, filtering, and washing obtained solid with cold water to give monohydrate of the title compound. MS(m/z):453(M++1). Calculated results (measured values) of element analysis for the product: C 53.62(53.58), H 5.36(5.48), and N 11.91(11.87).

Workup

  1. filtrationfiltering
  2. washwashing
  3. customobtained solid with cold water

Sources & evidence

ORD record
ord-2bfc6c5f5a754a858ff7c416aca353cc
Source dataset
uspto-grants-2010_07
Patent number
US07759362B2

Reaction notes

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