HCID 21072872, compound → HCID 178515246, compound

HRID 1372898Notes

Reaction equation

HRID 1372898 reaction equation
COC1C=CC(C[N:8]2[C:12]3[C:13](=[O:22])[C:14]4[CH:15]=[N:16][N:17]=[CH:18][C:19]=4[C:20](=[O:21])[C:11]=3[N:10]=[N:9]2)=CC=1>C(O)(C(F)(F)F)=O>[NH:8]1[C:12]2[C:13](=[O:22])[C:14]3[CH:15]=[N:16][N:17]=[CH:18][C:19]=3[C:20](=[O:21])[C:11]=2[N:10]=[N:9]1

Participants

3

Reactant 1

HCID 21072872HCID 21072872, compound

Product 1

HCID 178515246HCID 178515246, compoundYield 57.8%

Reagents, catalysts & solvents 1

HCID 6422Trifluoroacetic acidSolvent

Procedure

415 mg (1.29 mmol) of 1-(4-methoxybenzyl)-1H-[1,2,3]triazolo[4,5-g]phthalazin-4,9-dione was dissolved in 30 ml of TFA and refluxed for 2 days. TFA was removed under reduced pressure and 100 ml of 1M NaOH was added to residue, followed by washing with ethyl acetate. The resulting aqueous layer was acidified to pH 1 with HCl, and extracted with ethyl acetate. 150 mg of light brown powder was obtained by drying and concentrating the organic layer (yield 58%).

Workup

  1. temperaturerefluxed for 2 days
  2. customTFA was removed under reduced pressure and 100 ml of 1M NaOH
  3. additionwas added to residue
  4. washby washing with ethyl acetate
  5. extractionextracted with ethyl acetate

Sources & evidence

ORD record
ord-79bd5311e5d547f18557dada67c6a24b
Source dataset
uspto-grants-2007_01
Patent number
US07160884B2

Reaction notes

Loading…