Water → HCID 131733700, compound

HRID 706406Notes

Reaction equation

HRID 706406 reaction equation
O.O.O.[CH3:4][C@H:5]1[N:10]([CH2:11][C:12]([F:15])([F:14])[F:13])[C:9](=[O:16])[C@@H:8]([NH:17][C:18]([C:20]2[CH:21]=[C:22]3[CH2:37][C@@:27]4([C:35]5[C:30](=[N:31][CH:32]=[CH:33][CH:34]=5)[NH:29][C:28]4=[O:36])[CH2:26][C:23]3=[N:24][CH:25]=2)=[O:19])[CH2:7][C@H:6]1[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1.O.[C:45]([OH:54])(=[O:53])[C@@H:46]([C@H:48]([C:50]([OH:52])=[O:51])[OH:49])[OH:47]>C(#N)C>[C:45]([OH:54])(=[O:53])[C@@H:46]([C@H:48]([C:50]([OH:52])=[O:51])[OH:49])[OH:47].[CH3:4][C@H:5]1[N:10]([CH2:11][C:12]([F:15])([F:13])[F:14])[C:9](=[O:16])[C@@H:8]([NH:17][C:18]([C:20]2[CH:21]=[C:22]3[CH2:37][C@@:27]4([C:35]5[C:30](=[N:31][CH:32]=[CH:33][CH:34]=5)[NH:29][C:28]4=[O:36])[CH2:26][C:23]3=[N:24][CH:25]=2)=[O:19])[CH2:7][C@H:6]1[C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1

Participants

5

Reactant 3

HCID 962Water2×HCID 444305L-Tartaric acidHCID 1317336991488325-95-6

Product 1

HCID 131733700HCID 131733700, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

To suspension of 500 mg of (S)—N-((3S,5S,6R)-6-methyl-2-oxo-5-phenyl-1-(2,2,2-trifluoroethyl)piperidine-3-yl)-2′-oxo-1′,2′,5,7-tetrahydrospiro[cyclopenta[b]pyridine-6,3′-pyrrolo[2,3-b]pyridine]-3-carboxamide trihydrate in 5 mL of acetonitrile was added 5 mL of water slowly. ˜2 mL of addition of water, it became homogeneous. 124 mg of L-tartaric acid was added and sonicated followed by stirring for 3 hours. Crystalline materials was filtered and dried overnight at 40° C. yielding crystalline (S)—N-((3S,5S,6R)-6-methyl-2-oxo-5-phenyl-1-(2,2,2-trifluoroethyl)piperidine-3-yl)-2′-oxo-1′,2′,5,7-tetrahydrospiro[cyclopenta[b]pyridine-6,3′-pyrrolo[2,3-b]pyridine]-3-carboxamide L-tartaric acid cocrystal form.

Workup

  1. customsonicated
  2. filtrationCrystalline materials was filtered
  3. customdried overnight at 40° C.

Sources & evidence

ORD record
ord-0735897b91134bc0a6637121cbba535e
Source dataset
uspto-grants-2015_11
Patent number
US09174989B2

Reaction notes

Loading…