반응 #6949

반응 방정식

NaOH

cyanamide

3-benzyloxyphenylamine

HCl

→

N-(3-Benzyloxy-phenyl)guanidine

수율 98.4%

용매

1,4-dioxane

1,4-dioxane

반응 조건

후처리

1. 1
   온도then cooled to ambient temperature
2. 2
   여과the resulting precipitate was collected by filtration
3. 3
   기타The solid product was dried under vacuum overnight
4. 4
   기타to afford 23.8 g in 98.4% yield

실험 절차

To a suspension of 3-benzyloxyphenylamine (20.0 g, 100.35 mmol) in 1,4-dioxane (150 mL) was added cyanamide (7.39 g, 175.95 mmol followed by 4M HCl in 1,4-dioxane (44 ml, 176.00 mmol). The resulting suspension was heated at 80° C. overnight then cooled to ambient temperature and 6N NaOH (35 ml, 210.00 mmol) was added. The volume of solution was reduced to 50 ml in vacuo and the resulting precipitate was collected by filtration. The solid product was dried under vacuum overnight to afford 23.8 g in 98.4% yield. 1H NMR (MeOH-d4) δ 6.4–7.5 (m, 9H), 5.1 (s, 2H).

출처