Sodium Hydroxide → HCID 86740030, compound

HRID 1981101Notes

Reaction equation

HRID 1981101 reaction equation
COC([N:5]1[N:15](C(OC)=O)[CH:14]2[CH:6]1[CH:7]1[CH:20]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[C:12]3([CH2:13]2)[CH:8]1[N:9]=[N:10][N:11]3[C:26]1[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][CH:27]=1)=O.[OH-].[Na+].[O-]Cl.[Na+]>>[Cl:32][C:29]1[CH:30]=[CH:31][C:26]([N:11]2[N:10]=[N:9][CH:8]3[C:12]42[CH:20]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])[CH:7]3[CH:6]2[CH:14]([N:15]=[N:5]2)[CH2:13]4)=[CH:27][CH:28]=1

Participants

4

Reactant 3

HCID 14798Sodium HydroxideHCID 23665760Sodium HypochloriteHCID 54574901HCID 54574901, compound

Product 1

HCID 86740030HCID 86740030, compound

Conditions

Temperature
85 °C

Procedure

400 parts of 3,4-dimethoxycarbonyl-8-(4-chlorophenyl)-12-t-butoxy-3,4,8,9,10-pentazatetracyclo[5,4,1,02,5,07,11 ]dodec-9-ene (Compound No. 9) were suspended in 1,000 parts of 25 percent strength aqueous sodium hydroxide solution, and the suspension was stirred for 6 hours at 85° C. Thereafter, 1,150 parts of 13 percent strength aqueous NaOCl were added at 60° C. in the course of 2 hours, and stirring was continued for 4 hours at 60° C. The mixture was cooled to 20° C., after which the solid product was filtered off under suction, washed with 3,000 parts of water and dried at 30° C. under 1 mbar. 270 parts (96 mole %) of 8-(4-chlorophenyl)-12-t-butoxy-3,4,8,9,10-pentazatetracyclo[5,4,1,02,5,07,11 ]dodeca-3,9-diene of melting point 178° C. (decomposition) were obtained (Compound No. 2). ##STR21##

Workup

  1. stirringstirring
  2. waitwas continued for 4 hours at 60° C
  3. temperatureThe mixture was cooled to 20° C.
  4. filtrationafter which the solid product was filtered off under suction
  5. washwashed with 3,000 parts of water
  6. customdried at 30° C. under 1 mbar

Sources & evidence

ORD record
ord-d1f9832d59da472a8bc5e84c6744ff14
Source dataset
uspto-grants-1985_04
Patent number
US04512795

Reaction notes

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