反応 #1869156

反応方程式

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

溶媒

THF

THF

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   その他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
   ろ過The solid is filtered
5. 5
   洗浄washed with diisopropyl ether
6. 6
   その他dried in vacuo

実験手順

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.

出典