Lithium hydroxide, monohydrate → HCID 90229440, compound

HRID 1505803Notes

Reaction equation

HRID 1505803 reaction equation
[CH3:1][N:2]([CH3:18])[C:3]1[NH:7][C:6]2[CH:8]=[C:9]([N+:15]([O-:17])=[O:16])[CH:10]=[C:11]([C:12]([O-:14])=[O:13])[C:5]=2[N:4]=1.O.[OH-].[Li+]>C1COCC1.O>[CH3:1][N:2]([CH3:18])[C:3]1[NH:7][C:6]2[CH:8]=[C:9]([N+:15]([O-:17])=[O:16])[CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:5]=2[N:4]=1

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 90229441HCID 90229441, compound

Product 1

HCID 90229440HCID 90229440, compoundYield 91.6%

Reagents, catalysts & solvents 1

HCID 21881883Oxolane--water (1/1)Solvent

Procedure

2-(dimethylamino)-6-nitro-1H-benzimidazole-4-carboxylate (1.5 g) and lithium hydroxide hydrate (2.4 g) in THF—H2O (1:1, 100 mL) was stirred at 50° C. for 2 hours. THF was removed under reduced pressure, and 1N hydrochloric acid was added to the residue with stirring under ice-cooling to adjust the pH to 5. The precipitate was collected by filtration and dried under reduced pressure to obtain the titled compound (1.38 g) as yellow solid.

Workup

  1. customTHF was removed under reduced pressure, and 1N hydrochloric acid
  2. additionwas added to the residue
  3. temperaturecooling
  4. filtrationThe precipitate was collected by filtration
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-ba76446889a3433baf1e93f2be2dd053
Source dataset
uspto-grants-2015_12
Patent number
US09216968B2

Reaction notes

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