反应 #1869156

反应方程式

TFA (D)Arg-(D)Nle-(D)Nle-(D)Nle-(D)Arg-(D)Nle-(D)Nle-(D)Nle-Gly-(D)Tyr-NH2

phenol

toluene

TFA

→

Boc-Gly-(D)Tyr-NH2

溶剂

THF

THF

反应条件

后处理

1. 1
   浓缩concentrated in vacuo
2. 2
   其他Residual TFA is removed by azeotropic distillation with toluene
3. 3
   workup.ADDITIONThe residue is poured into a mixture of petroleum ether and diisopropyl ether
4. 4
   过滤The solid is filtered
5. 5
   洗涤washed with diisopropyl ether
6. 6
   其他dried in vacuo

实验过程

The deprotected peptide SF1257-13 (TFA-(D)Arg-(D)Nle-(D)Nle-(D)Nle-(D)Arg-(D)Nle-(D)Nle-(D)Nle-Gly-(D)Tyr-NH2 (SEQ ID NO:1) is made by slowly adding TFA (A×3 l) to a mixture of SF1257-12 (A kg) and phenol (A×0.1 kg) in toluene and THF while maintaining the temperature at ≦18° C. The reaction mixture is allowed to warm up to room temperature. Following completion of cleavage, the solvent is diluted with THF and then concentrated in vacuo. Residual TFA is removed by azeotropic distillation with toluene. The residue is poured into a mixture of petroleum ether and diisopropyl ether. The solid is filtered, washed with diisopropyl ether and dried in vacuo.

来源