Ammonia → HCID 12109530, compound

HRID 478847Notes

Reaction equation

HRID 478847 reaction equation
[CH:1]1([N:7]([CH3:22])[C:8]([C:10]2[S:21][C:13]3=[N:14][C:15]4[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=4[N:12]3[CH:11]=2)=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[N+:23]([O-])([OH:25])=[O:24].N>S(=O)(=O)(O)O>[CH:1]1([N:7]([CH3:22])[C:8]([C:10]2[S:21][C:13]3=[N:14][C:15]4[CH:20]=[CH:19][C:18]([N+:23]([O-:25])=[O:24])=[CH:17][C:16]=4[N:12]3[CH:11]=2)=[O:9])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 222AmmoniaHCID 944Nitric AcidHCID 9926839HCID 9926839, compound

Product 1

HCID 12109530HCID 12109530, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

The compound of Example 3 (12.3 g) was dissolved in concentrated sulfuric acid, and this was mixed with fuming nitric acid (1.95 ml) under ice-cooling and then stirred at room temperature for 30 minutes. The reaction solution was poured into ice water and neutralized by adding saturated NH3 aqueous solution, and then the thus formed precipitate was collected by filtration. The thus collected crude crystals were washed with hot MeOH to obtain the title compound (12.7 g).

Workup

  1. temperaturecooling
  2. filtrationthe thus formed precipitate was collected by filtration
  3. customThe thus collected crude crystals
  4. washwere washed with hot MeOH

Sources & evidence

ORD record
ord-799722c2707040ba9ed67a1bd6573451
Source dataset
uspto-grants-2003_11
Patent number
US06642264B1

Reaction notes

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