Nitric Acid → HCID 18789079, compound

HRID 1586054Notes

Reaction equation

HRID 1586054 reaction equation
S(=O)(=O)(O)O.[Cl:6][CH2:7][CH2:8][C:9]1[C:10]([Cl:19])=[N:11][C:12]2[N:13]([N:16]=[CH:17][CH:18]=2)[C:14]=1[Cl:15].[N+:20]([O-])([OH:22])=[O:21]>>[Cl:6][CH2:7][CH2:8][C:9]1[C:10]([Cl:19])=[N:11][C:12]2[N:13]([N:16]=[CH:17][C:18]=2[N+:20]([O-:22])=[O:21])[C:14]=1[Cl:15]

Participants

4

Reactant 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 18789177HCID 18789177, compound

Product 1

HCID 18789079HCID 18789079, compoundYield 95.5%

Conditions

Temperature
0 °C

Procedure

To 100 ml of concentrated sulfuric acid cooled to 0° C. with ice water, were added 50 ml of 90% nitric acid gradually so as not to raise the temperature. After the resultant mixed acid was stirred for a while, 13.80 g of the compound prepared in Example 49 as remained crystals were added gradually so as not to raise the temperature also. The resultant mixture was stirred for 4 hours while maintaining the temperature at 0° C. Since spots attributable to the raw materials on TLC disappeared, the stirring was stopped, and the reaction mixture was poured into ice water. Crystals deposited were collected by filtration and air-dried to obtain 15.61 g (yield: 95.5%) of the intended product. Yellow crystals.

Workup

  1. temperatureto raise the temperature
  2. additionAfter the resultant mixed acid
  3. additionwere added gradually so as not
  4. temperatureto raise the temperature also
  5. filtrationCrystals deposited were collected by filtration
  6. customair-dried

Sources & evidence

ORD record
ord-deeae2db037248b09458789e33d44178
Source dataset
uspto-grants-1999_08
Patent number
US05942515

Reaction notes

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