Lithium hydroxide, monohydrate → HCID 67954954, compound

HRID 1258880Notes

Reaction equation

HRID 1258880 reaction equation
O.[OH-].[Li+].C[O:5][C:6](=[O:31])[C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH:17]=[C:16]([C:18]3[N:19]([CH3:30])[N:20]=[N:21][C:22]=3[C:23]3[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=3)[N:15]=[CH:14]2)=[CH:9][CH:8]=1>O.C1COCC1.CO>[F:29][C:26]1[CH:27]=[CH:28][C:23]([C:22]2[N:21]=[N:20][N:19]([CH3:30])[C:18]=2[C:16]2[N:15]=[CH:14][N:13]([C:10]3[CH:9]=[CH:8][C:7]([C:6]([OH:31])=[O:5])=[CH:12][CH:11]=3)[CH:17]=2)=[CH:24][CH:25]=1

Participants

6

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 57378559HCID 57378559, compound

Product 1

HCID 67954954HCID 67954954, compoundYield 86%

Reagents, catalysts & solvents 3

HCID 887MethanolSolventHCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of lithium hydroxide monohydrate (85 mg, 2.01 mmol) in water (2.5 mL) was added dropwise to a suspension of 4-{4-[5-(4-fluoro-phenyl)-3-methyl-3H-[1,2,3]triazol-4-yl]-imidazol-1-yl}-benzoic acid methyl ester (380 mg, 1.01 mmol) in THF (2.5 mL) and methanol (0.5 mL). The reaction mixture was then stirred at room temperature for 1 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 (315 mg, 86%) as a white solid. MS: m/e=362.3 [M−H]−.

Workup

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

Sources & evidence

ORD record
ord-4eb3a450b3984a09a5f9229497a060cc
Source dataset
uspto-grants-2013_06
Patent number
US08466181B2

Reaction notes

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