تفاعل #3843

معادلة التفاعل

Ethyl acetate

[2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone

Hydroxylamine hydrochloride

HCl

→

title compound

المردود 35.9%

{2-[2-(hydroxyimino-phenyl-methyl)-phenyldisulfanyl]phenyl}-phenyl-methanon

المردود 35.9%

المذيبات

ethanol

pyridine

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe solution was refluxed for 90 minutes
2. 2
   درجة الحرارةThe solution was cooled
3. 3
   أخرىthe layers were separated
4. 4
   غسيلthe organic portion was washed with brine
5. 5
   تجفيفdried (MgSO4)
6. 6
   ترشيحfiltered
7. 7
   تركيزThe filtrate was concentrated to dryness
8. 8
   أخرىthe residue was triturated with 75% hexane/25% ethyl acetate

الإجراء التجريبي

The [2-(2-benzoyl-phenyldisulfanyl)-phenyl]phenyl-methanone (0.55 g, 1.2 mmol) was diluted with ethanol (5 mL) and anhydrous pyridine (5 mL). Hydroxylamine hydrochloride (1 g, 14 mmol) was added and the solution was refluxed for 90 minutes. The solution was cooled and poured into cold aqueous HCl (1N). Ethyl acetate was added, the layers were separated, and the organic portion was washed with brine, dried (MgSO4), and filtered. The filtrate was concentrated to dryness and the residue was triturated with 75% hexane/25% ethyl acetate to give the title compound (0.19 g, 32%) as a white solid, mp 191°-193° C.;

المصدر