HCID 14025254, compound → HCID 66881691, compound

HRID 1893562Notes

Reaction equation

HRID 1893562 reaction equation
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH3:11])=[CH:10][C:5]=2[O:4][C:3]1=[O:12].[N:13]([O-:15])=[O:14].[Na+]>FC(F)(F)C(O)=O>[CH3:1][N:2]1[C:6]2[CH:7]=[C:8]([N+:13]([O-:15])=[O:14])[C:9]([CH3:11])=[CH:10][C:5]=2[O:4][C:3]1=[O:12]

Participants

4

Reactant 2

HCID 14025254HCID 14025254, compoundHCID 23668193Sodium Nitrite

Product 1

HCID 66881691HCID 66881691, compoundYield 65%

Reagents, catalysts & solvents 1

HCID 6422Trifluoroacetic acidSolvent

Procedure

The compound (3.33 g, 20.4 mmol) obtained in step A was dissolved in trifluoroacetic acid (60 ml), sodium nitrite (1.41 g, 20.4 mmol) was gradually added under ice-cooling with stirring, and the mixture was stirred at room temperature for 3 hr. The reaction solution was poured into ice water, and the precipitated solid was collected by filtration, washed with water, and dried under reduced pressure to give the title compound (2.75 g, yield 65%) as a pale-bistered solid.

Workup

  1. temperaturecooling
  2. stirringthe mixture was stirred at room temperature for 3 hr
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with water
  5. customdried under reduced pressure

Sources & evidence

ORD record
ord-dacbb68ab2c947caaa066c52a8225146
Source dataset
uspto-grants-2013_08
Patent number
US08513235B2

Reaction notes

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