تفاعل #334538

معادلة التفاعل

Oxalic acid

hydroxylamine

H2SO4

→

hydroxylammonium oxalate

المردود 94.6%

المذيبات

methanol

methanol

ظروف التفاعل

المعالجة

1. 1
   أخرىthe thin white precipitat
2. 2
   أخرىformed
3. 3
   ترشيحwas filtered off
4. 4
   workup.ADDITIONA magnetic stirring bar was introduced
5. 5
   أخرىthe flask was placed in an ice-water bath
6. 6
   workup.ADDITIONwas slowly added
7. 7
   درجة الحرارةwith cooling
8. 8
   أخرىA thick white slurry was produced
9. 9
   ترشيحthis was filtered
10. 10
    أخرىthe crude white solid (84.8 g) was collected
11. 11
    أخرىA portion (25 g) of this solid was recrystallized from hot water

الإجراء التجريبي

A solution of hydroxylamine in methanol (680 mL) as in Example 27 was used (pH 11.8). Conc. H2SO4 was slowly added to adjust the pH to 8.0 and the thin white precipitat formed was filtered off and the clear filtrate placed in a 1 liter Erlenmeyer flask. A magnetic stirring bar was introduced and the flask was placed in an ice-water bath. Oxalic acid (45 g; 0.5 mol) dissolved in methanol (100 mL) was slowly added with cooling and stirring. A thick white slurry was produced and this was filtered and the crude white solid (84.8 g) was collected. A portion (25 g) of this solid was recrystallized from hot water to produce white crystalline hydroxylammonium oxalate (M.P. 192° C. with decomposition). Yield 94.6%.

المصدر