Hydroxyamine hydrochloride → HCID 86741357, compound

HRID 1252296Notes

Reaction equation

HRID 1252296 reaction equation
[Cl:1][C:2]1[C:3]2[C:4](=[O:16])[CH:5]3[CH2:14][CH2:13][C:12](=O)[N:6]3[CH2:7][C:8]=2[CH:9]=[CH:10][CH:11]=1.[OH2:17].O.O.C([O-])(=O)C.[Na+].Cl.[NH2:26]O>C(O)C.O>[Cl:1][C:2]1[C:3]2[C:4](=[O:16])[CH:5]3[CH2:14][CH2:13][C:12](=[N:26][OH:17])[N:6]3[CH2:7][C:8]=2[CH:9]=[CH:10][CH:11]=1

Participants

6

Reactant 3

HCID 443297Hydroxyamine hydrochlorideHCID 13662503HCID 13662503, compoundHCID 23665404Sodium Acetate Trihydrate

Product 1

HCID 86741357HCID 86741357, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent2×

Procedure

A suspension of 1.00 g of 9-chloro-1,10a-dihydropyrrolo[1,2-b]isoquinoline-3,10[2H,5H]-dione in 95% ethanol (10 ml) was treated with a premixed solution prepared from 1.17 g of sodium acetate trihydrate in water (5 ml) and 0.60 g of hydroxylamine hydrochloride in water (5 ml). The suspension was heated in reflux and after 15 minutes a solution formed. After 1 hour of reflux, a precipitate began to form. Heating was continued for another 1.5 hours, after which time the mixture was allowed to cool to ambient temperature. The precipitate was isolated by vacuum filtration and dried under vacuum at 40° C.

Workup

  1. additionwas treated with a premixed solution
  2. temperatureThe suspension was heated
  3. temperaturein reflux and after 15 minutes a solution
  4. customformed
  5. temperatureAfter 1 hour of reflux
  6. customto form
  7. temperatureHeating
  8. customThe precipitate was isolated by vacuum filtration
  9. customdried under vacuum at 40° C.

Sources & evidence

ORD record
ord-60c74e68b9564d56ac82f0127295f32d
Source dataset
uspto-grants-1988_05
Patent number
US04742171

Reaction notes

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