HRID1649340
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
PROCEDURE
实验过程
In 80% acetic acid (20 ml) was suspended Tr-Trp(Tos)-OBzl (1.3 g, 1.88 mM) and the mixture was stirred at room temperature for one hour, whereby the material was dissolved. The precipitated triphenylmethanol was filtered off and the filtrate was subjected to catalytic reduction for 4 hours in the presence of palladium black at room temperature. The catalyst was filtered off and the acetic acid was distilled off. The residue was recrystallized from water to give H-Trp(Tos)-OH. Yield 585 mg (86.9%); m.p. 227° C. (decomp.); [α]D21 -29.2° (c=0.5, acetic acid).
WORKUP
后处理
- dissolutionwhereby the material was dissolved
- filtrationThe precipitated triphenylmethanol was filtered off
- waitthe filtrate was subjected to catalytic reduction for 4 hours in the presence of palladium black at room temperature
- filtrationThe catalyst was filtered off
- distillationthe acetic acid was distilled off
- customThe residue was recrystallized from water