반응 #685035
ord-f34e2230563a4c58af21ea9555077c17
반응 방정식
hydrogen chloride
tert-butyl 2-(4-methoxybenzyl)hydrazinecarboxylate
→
title compound
수율 98.0%
(4-Methoxybenzyl)hydrazine dihydrochloride
수율 98.0%
반응 조건
온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타Collect the solids
- 2여과by filtration
- 3기타isolate the solids
- 4여과by filtration
- 5기타Dry the solids
실험 절차
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).