反応 #3843

反応方程式

Ethyl acetate

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

Hydroxylamine hydrochloride

HCl

→

title compound

収率 35.9%

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

収率 35.9%

溶媒

ethanol

pyridine

反応条件

後処理

1. 1
   温度the solution was refluxed for 90 minutes
2. 2
   温度The solution was cooled
3. 3
   その他the layers were separated
4. 4
   洗浄the organic portion was washed with brine
5. 5
   乾燥dried (MgSO4)
6. 6
   ろ過filtered
7. 7
   濃縮The filtrate was concentrated to dryness
8. 8
   その他the residue was triturated with 75% hexane/25% ethyl acetate

実験手順

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.;

出典