Hydrogen Peroxide → HCID 86740031, compound

HRID 1981102Notes

Reaction equation

HRID 1981102 reaction equation
OO.[Br:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[N:20]=[N:19][CH:18]3[C:11]42[CH:21]([OH:22])[CH:17]3[CH:16]2[CH:13]([NH:14][NH:15]2)[CH2:12]4)=[CH:6][CH:5]=1.CO.[OH-].[Na+]>O>[Br:3][C:4]1[CH:9]=[CH:8][C:7]([N:10]2[N:20]=[N:19][CH:18]3[C:11]42[CH:21]([OH:22])[CH:17]3[CH:16]2[CH:13]([N:14]=[N:15]2)[CH2:12]4)=[CH:6][CH:5]=1

Participants

6

Reactant 4

HCID 784Hydrogen PeroxideHCID 887MethanolHCID 14798Sodium HydroxideHCID 57297197HCID 57297197, compound

Product 1

HCID 86740031HCID 86740031, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
20 °C

Procedure

35 parts of 30 percent strength aqueous H2O2 were added dropwise, in the course of 1 hour, to 50 parts of 8-(4-bromophenyl)-12-hydroxy-3,4,8,9,10-pentazatetracyclo[5,4,1,02,5,07,11 ]dodec-9ene (Compound No. 69) in 400 parts of methanol and 5 parts of 25 percent strength by weight aqueous NaOH, at 65° C., while stirring, and stirring was continued for 5 hours at 65° C. The mixture was cooled to 20° C., after which 1,500 parts of water were added, and the product was filtered off under suction, washed with 300 parts of water and dried at 30° C. under 1 mbar. 44 parts (88 mole %) of 8-(4-bromophenyl)-12hydroxy-3,4,8,9,10-pentazatetracyclo[5,4,1,02,5,07,11 ]-dodeca-3,9-diene of melting point 187° C. (decomposition) were obtained (Compound No. 3).

Workup

  1. filtrationthe product was filtered off under suction
  2. washwashed with 300 parts of water
  3. customdried at 30° C. under 1 mbar

Sources & evidence

ORD record
ord-7fb0b012a612421d8d40a5bc8ba4a2c0
Source dataset
uspto-grants-1985_04
Patent number
US04512795

Reaction notes

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