Nitric Acid → HCID 14817081, compound

HRID 373444Notes

Reaction equation

HRID 373444 reaction equation
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:14])[CH3:13])=[CH:7][C:6]=1[F:15])(=[O:3])[CH3:2].[N+:16]([O-])([OH:18])=[O:17]>C(O)(=O)C>[C:1]([NH:4][C:5]1[CH:10]=[C:9]([N+:16]([O-:18])=[O:17])[C:8]([NH:11][C:12](=[O:14])[CH3:13])=[CH:7][C:6]=1[F:15])(=[O:3])[CH3:2]

Participants

4

Reactant 2

HCID 944Nitric AcidHCID 148170801,4-Bisacetylamino-2-fluorobenzene

Product 1

HCID 14817081HCID 14817081, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent2×

Conditions

Temperature
40 °C

Procedure

157.5 g (0.75 mol) of the 1,4-bisacetylamino-2-fluorobenzene obtained above under B. are initially introduced into 630 g of glacial acetic acid, and a mixture of 42 g of glacial acetic acid and 51 g of nitric acid (density 1.5) is added dropwise in the course of 2 hours. The mixture is subsequently stirred at 40° C. for a further 2 hours and cooled to 15° C. After the product which has precipitated has been filtered off, it is washed twice with 50 ml of glacial acetic acid each time and dried at 50° C. in a vacuum cabinet.

Workup

  1. additionis added dropwise in the course of 2 hours
  2. temperaturecooled to 15° C
  3. customAfter the product which has precipitated
  4. filtrationhas been filtered off
  5. washit is washed twice with 50 ml of glacial acetic acid each time
  6. customdried at 50° C. in a vacuum cabinet

Sources & evidence

ORD record
ord-dca34d19e2db408d81b64814efeffab2
Source dataset
uspto-grants-1992_11
Patent number
US05163970

Reaction notes

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