تفاعل #685035

معادلة التفاعل

hydrogen chloride

tert-butyl 2-(4-methoxybenzyl)hydrazinecarboxylate

→

title compound

المردود 98.0%

(4-Methoxybenzyl)hydrazine dihydrochloride

المردود 98.0%

المذيبات

dioxane

dioxane

ظروف التفاعل

المعالجة

1. 1
   أخرىCollect the solids
2. 2
   ترشيحby filtration
3. 3
   أخرىisolate the solids
4. 4
   ترشيحby filtration
5. 5
   أخرىDry the solids

الإجراء التجريبي

To a solution of 4 N hydrogen chloride in dioxane (2000 mL, 8.00 mol HCl), add tert-butyl 2-(4-methoxybenzyl)hydrazinecarboxylate (324 g, 1.09 mol) dissolved in a minimal amount of dioxane, slowly over a period of 1 h. A precipitate gradually forms. Allow the solution to stir 16 h at 20±5° C. Collect the solids by filtration. Slurry the solids in heptane (2000 mL) and isolate the solids by filtration. Dry the solids using a nitrogen press to give the title compound (242.3 g, 1.08 mol, 98%). 1H NMR (400 MHz, DMSO-d6) δ 8.2-9.0 (bs, 5H), 7.3-7.4 (d, 2H), 6.8-7.0 (d, 2H), 4.0 (s, 2H), 3.7 (s, 3H).

المصدر