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Sodium Hydroxide → HCID 178432262, compound

HRID 513872
Notes
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Reaction equation

HRID 513872 reaction equation
[NH2:1][C:2]1[N:6]([C:7]2[CH:16]=[CH:15][C:10]3[NH:11][C:12]([CH3:14])=[N:13][C:9]=3[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:17]([C:19]1[N:20](CC2C=CC(OC)=CC=2)[C:21]([Br:25])=[C:22]([Br:24])[CH:23]=1)=[O:18].[OH-].[Na+]>C(OCC)(=O)C.S(=O)(=O)(O)O>[NH2:1][C:2]1[N:6]([C:7]2[CH:16]=[CH:15][C:10]3[NH:11][C:12]([CH3:14])=[N:13][C:9]=3[CH:8]=2)[N:5]=[CH:4][C:3]=1[C:17]([C:19]1[NH:20][C:21]([Br:25])=[C:22]([Br:24])[CH:23]=1)=[O:18]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 178490813HCID 178490813, compound

Product 1

HCID 178432262HCID 178432262, compound

Reagents, catalysts & solvents 1

HCID 86628183Ethyl acetate sulfuric acidSolvent

Conditions

Temperature
80 °C

Procedure

[5-Amino-1-(2-methyl-1H-benzimidazol-5-yl)-1H-pyrazol-4-yl]-[4,5-dibromo-1-(4-methoxy-benzyl)-1H-pyrrol-2-yl]-methanone (317 mg) was dissolved in ethyl acetate/sulfuric acid (4/1; 5 ml). This was stirred at 80° C. for four hours. The pH of the reaction mixture was adjusted to 11 (basic) using an aqueous solution of 5 M sodium hydroxide while cooling it on ice. The reaction mixture was extracted with ethyl acetate/tetrahydrofuran (THF) (10 ml). The organic layer was washed with an aqueous solution saturated with sodium chloride (5 ml), and the organic layer was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (dichloromethane/methanol). Thus, a brown solid was obtained (135 mg, 54%).

Workup

  1. temperaturewhile cooling it on ice
  2. extractionThe reaction mixture was extracted with ethyl acetate/tetrahydrofuran (THF) (10 ml)
  3. washThe organic layer was washed with an aqueous solution saturated with sodium chloride (5 ml)
  4. concentrationthe organic layer was concentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (dichloromethane/methanol)
  6. customThus, a brown solid was obtained (135 mg, 54%)

Sources & evidence

ORD record
ord-a4b890b95863479e85badeb176166004
Source dataset
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09102692B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes