HomeMCPWorkbenchSkills
HomeWorkbenchNotificationsMe
llms.txt · MCP GuidePrivacy Policy · Terms of Service · Supportv1.8.0
  1. Home
  2. /Reaction

Ethyl Acetate → 4-Acetamino-2-cyanobiphenyl

HRID 866229
Notes
Print preview

Reaction equation

HRID 866229 reaction equation
[C:1]([C:3]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)#[N:2].[C:18](OCC)(=[O:20])[CH3:19]>[Pd]>[NH:9]([C:7]1[CH:6]=[CH:5][C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:3]([C:1]#[N:2])[CH:8]=1)[C:18]([CH3:19])=[O:20]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 8857Ethyl AcetateHCID 214689572-Cyano-4-nitrobiphenyl

Product 1

HCID 214688684-Acetamino-2-cyanobiphenyl

Reagents, catalysts & solvents 1

HCID 23938PalladiumCatalyst

Procedure

2-Cyano-4-nitrobiphenyl (0.067 moles, 15.0 g.) was dissolved in 100 ml ethyl acetate/100 ml ethanol and hydrogenated at 40 psi over 3.0 g of 10% palladium on carbon. The catalyst was removed by filtering though celite. The solvents were removed in vacuo. The residue was dissolved in 175 ml of methylene chloride. Acetic anhydride (15 ml) was added. The reaction was stirred at room temperature for 30 minutes and poured over ice. The organic layer was dried, concentrated, and then purified by HPLC over silica gel eluted with a gradient of 0-10% ethyl acetate in chloroform. (MS)

Workup

  1. customThe catalyst was removed
  2. filtrationby filtering though celite
  3. customThe solvents were removed in vacuo
  4. dissolutionThe residue was dissolved in 175 ml of methylene chloride
  5. additionAcetic anhydride (15 ml) was added
  6. additionpoured over ice
  7. customThe organic layer was dried
  8. concentrationconcentrated
  9. custompurified by HPLC over silica gel
  10. washeluted with a gradient of 0-10% ethyl acetate in chloroform

Sources & evidence

ORD record
ord-1734f169399740cfa3116dab0fcf16e1
Source dataset
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US05569768

Reaction notes

Loading…

On this pageParticipantsProcedureWorkupSources & evidenceReaction notes