Lithium hydroxide, monohydrate → HCID 57378905, compound

HRID 1258896Notes

Reaction equation

HRID 1258896 reaction equation
O.[OH-].[Li+].[F:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[N:12]=[N:13][N:14]([CH3:31])[C:15]=1[C:16]1[N:17]=[CH:18][N:19]([C:21]2[CH:30]=[CH:29][C:24]([C:25]([O:27]C)=[O:26])=[CH:23][N:22]=2)[CH:20]=1>O.C1COCC1.CO>[F:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[N:12]=[N:13][N:14]([CH3:31])[C:15]=1[C:16]1[N:17]=[CH:18][N:19]([C:21]2[CH:30]=[CH:29][C:24]([C:25]([OH:27])=[O:26])=[CH:23][N:22]=2)[CH:20]=1

Participants

6

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 57378904HCID 57378904, compound

Product 1

HCID 57378905HCID 57378905, compoundYield 90%

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of lithium hydroxide monohydrate (63 mg, 1.49 mmol) in water (3.0 mL) was added dropwise to a suspension of methyl 6-(4-(4-(2-fluorophenyl)-1-methyl-1H-1,2,3-triazol-5-yl)-1H-imidazol-1-yl)nicotinate (282 mg, 0.745 mmol) in THF (6.0 mL) and methanol (1 mL). The reaction mixture was then stirred at room temperature for 1.5 h and was then evaporated and the residue dissolved in water, acidified with HCl (1 N), and the resulting precipitate filtered off to afford the title product (244 mg, 90%) as a white solid. MS: m/e=363.3 [M−H]−.

Workup

  1. customwas then evaporated
  2. dissolutionthe residue dissolved in water
  3. filtrationthe resulting precipitate filtered off

Sources & evidence

ORD record
ord-d3d90c3783bf43b9a0fee1159f1a104f
Source dataset
uspto-grants-2013_06
Patent number
US08466181B2

Reaction notes

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