Lithium hydroxide, monohydrate → HCID 67498530, compound

HRID 402398Notes

Reaction equation

HRID 402398 reaction equation
O.[OH-].[Li+].C([O:6][C:7]([C:9]1[N:10]=[N:11][C:12]([O:15][CH2:16][C:17]2[N:18]([CH3:29])[N:19]=[N:20][C:21]=2[C:22]2[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=2)=[CH:13][CH:14]=1)=[O:8])C>O.C1COCC1>[F:28][C:25]1[CH:24]=[CH:23][C:22]([C:21]2[N:20]=[N:19][N:18]([CH3:29])[C:17]=2[CH2:16][O:15][C:12]2[N:11]=[N:10][C:9]([C:7]([OH:8])=[O:6])=[CH:14][CH:13]=2)=[CH:27][CH:26]=1

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 57334945HCID 57334945, compound

Product 1

HCID 67498530HCID 67498530, compoundYield 99%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of lithium hydroxide monohydrate (111 mg, 3.09 mmol) in water (5 mL) was added dropwise to a suspension of 6-[5-(4-fluoro-phenyl)-3-methyl-3H-[1,2,3]triazol-4-ylmethoxy]-pyridazine-3-carboxylic acid ethyl ester (471 mg, 1.32 mmol) in THF (5 mL). The reaction mixture was then stirred at room temperature for 16 h. The reaction mixture was then evaporated and the residue dissolved in water, acidified with HCl (1N), and the resulting precipitate filtered off to afford the title product (430 mg, 99%) as a white solid after trituration with ethyl acetate. MS: m/e=328.3 [M−H]−.

Workup

  1. customThe reaction mixture was then evaporated
  2. dissolutionthe residue dissolved in water
  3. filtrationthe resulting precipitate filtered off

Sources & evidence

ORD record
ord-9160003ff92c4bc1b02ba6fcd5767f8d
Source dataset
uspto-grants-2014_06
Patent number
US08742097B2

Reaction notes

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