反应详情

To a solution of 1.84 g of sodium in 80 ml of methanol is added, at 50°, a solution of 1.82 g of hydroxylamine hydrochloride in 30 ml of methanol. To the suspension is added, with stirring, a solution of 5.8 g of [o-(2,6-dichloroanilino)-phenyl]-acetamide (M.P. 188°-189°) in 80 ml of methanol, and the whole subsequently refluxed for 18 hours. After cooling, the red suspension is concentrated at 40° under 11 Torr to dryness. The residue is shaken with 600 ml of water and 100 ml of ether. The aqueous phase is separated and acidified with 2 N hydrochloric acid. The suspension is extracted with 200 ml of ether, the ether solution separated, washed with water, dried over magnesium sulphate, and concentrated at 40° under 11 Torr. The residue is crystallized from ether, whereby [o-(2,6-dichloroanilino)-phenyl]-acetohydroxamic acid is obtained, M.P. 164°-165°.

1. additionTo the suspension is added
2. temperatureAfter cooling
3. concentrationthe red suspension is concentrated at 40° under 11 Torr to dryness
4. stirringThe residue is shaken with 600 ml of water and 100 ml of ether
5. customThe aqueous phase is separated
6. extractionThe suspension is extracted with 200 ml of ether
7. customthe ether solution separated
8. washwashed with water
9. dry with materialdried over magnesium sulphate
10. concentrationconcentrated at 40° under 11 Torr
11. customThe residue is crystallized from ether