Hydroxyamine hydrochloride → HCID 131722394, compound
Reaction equation
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[O:10][C:9]([CH3:15])([CH3:14])[C:8](=O)[CH2:7]2)([OH:3])=[O:2].Cl.[NH2:18][OH:19]>C(O)C.N1C=CC=CC=1>[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[O:10][C:9]([CH3:15])([CH3:14])[CH2:8][C:7]2=[N:18][OH:19])([OH:3])=[O:2]Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Conditions
- Temperature
- 80 °C
Procedure
14.9 g of 6-carboxy-2,2-dimethyl-3-chromanone are dissolved in 100 ml of ethanol and 100 ml of pyridine, and after addition of 5.16 g of hydroxylamine hydrochloride the mixture is heated at 80° C. with stirring for 6 hours. The solvent is distilled off on a rotary evaporator. The residue is treated with water and adjusted to pH<1 using conc. hydrochloric acid, and the colorless crystals are filtered off.
Workup
- distillationThe solvent is distilled off on a rotary evaporator
- additionThe residue is treated with water
- filtrationthe colorless crystals are filtered off
Sources & evidence
- ORD record
- ord-d452c6351e804a80bddc69fe5df7cc03
- Source dataset
- uspto-grants-2001_02
- Patent number
- US06191164B1
Reaction notes
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