Hydroxyamine hydrochloride → HCID 86741357, compound

HRID 652242Notes

Reaction equation

HRID 652242 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 to 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. temperatureto 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-bfa6225f43344206bac69d91db459fc1
Source dataset
uspto-grants-1987_06
Patent number
US04670562

Reaction notes

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