HRID1249296
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- -15 °C
PROCEDURE
实验过程
A solution of 4-(2,4-dinitrophenoxy)-phenyldiazomethane in CH2Cl2 (20 ml) is added to a solution of Boc-dehydroalanine-p-nitrobenzyl ester (2) in 20 ml CH2Cl2 at -15° C. After stirring 1 hr at -15° C. and 4 hr at 25°, the solution is evaporated to dryness and the residue is triturated with hexane. The solid product, p-nitrobenzyl 3-t-butoxycarbonylamino-5-(4-[2,4-dinitrophenoxyl]-phenyl)-pyrazoline-3-carboxylate (18), is recrystallized from ethyl acetate-hexane to constant melting point. NMR (CDCl3)δ: 4.8-5.4 (m, 1H, CH--N=N).
WORKUP
后处理
- customthe solution is evaporated to dryness
- customthe residue is triturated with hexane
- customThe solid product, p-nitrobenzyl 3-t-butoxycarbonylamino-5-(4-[2,4-dinitrophenoxyl]-phenyl)-pyrazoline-3-carboxylate (18), is recrystallized from ethyl acetate-hexane