Hydrochloric Acid → HCID 66839107, compound

HRID 599596Notes

Reaction equation

HRID 599596 reaction equation
[OH2:1].[OH-].[Li+].[F:4][C:5]1[CH:12]=[C:11]([N:13]2[CH:17]=[C:16]([CH3:18])[N:15]=[CH:14]2)[C:10]([O:19][CH3:20])=[CH:9][C:6]=1[CH:7]=O.[OH-].[Na+].Cl.[CH2:24]1[CH2:28][O:27]CC1>C(O)C>[F:4][C:5]1[CH:12]=[C:11]([N:13]2[CH:17]=[C:16]([CH3:18])[N:15]=[CH:14]2)[C:10]([O:19][CH3:20])=[CH:9][C:6]=1/[CH:7]=[CH:24]/[C:28]([OH:1])=[O:27]

Participants

7

Reactant 5

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 168937Lithium hydroxide, monohydrateHCID 73014035HCID 73014035, compound

Product 1

HCID 66839107HCID 66839107, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Lithium hydroxide monohydrate (240 mg) was added to a mixed solution of 2-fluoro-5-methoxy-4-(4-methyl-1H-imidazol-1-yl)benzaldehyde (CAS No. 870851-52-8, 1.03 g) and triethyl phosphonoacetate (1.09 g) in THF (4 mL) and ethanol (1 mL), and the reaction solution was stirred at room temperature for five hours. A 2 N sodium hydroxide solution (4 mL) was added to the reaction solution, and the reaction solution was stirred for 17 hours. 2 N aqueous hydrochloric acid (4 mL) was added to the reaction solution, and the reaction solution was stirred at room temperature for 30 minutes. Then, the precipitated solid was collected by filtration and washed with water and an ether. The resulting solid was air-dried to obtain 1.03 g of the title compound. The property value of the compound is as follows.

Workup

  1. stirringthe reaction solution was stirred at room temperature for 30 minutes
  2. filtrationThen, the precipitated solid was collected by filtration
  3. washwashed with water
  4. customThe resulting solid was air-dried

Sources & evidence

ORD record
ord-d6814309b77440308bfab9e88b3e132b
Source dataset
uspto-grants-2011_03
Patent number
US07897632B2

Reaction notes

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