反应 #84045
ord-a1fc588f2049422e98b62bbc955960d0
反应方程式
N-Boc-1,6-diaminohexane
Fmoc-Phe-Gly-OH
N,N′-dicyclohexylcarbodiimide
1-hydroxybenzotriazole hydrate
→
Fmoc-Phe-Gly-NH—(CH2)6NH-Boc
收率 94.3%
反应物
试剂
无
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1workup.STIRRINGstirred overnight
- 2过滤Solids were filtered off
- 3洗涤they were washed with EtOAc
- 4浓缩The filtrate and washings were then concentrated under reduced pressure
- 5其他The resulting residue was purified by flash column chromatography (0 to 10% MeOH in CH2Cl2)
实验过程
To a solution of Fmoc-Phe-Gly-OH (0.66 g) in anhydrous THF (20 mL) at 0° C. under N2 was added N,N′-dicyclohexylcarbodiimide (0.307 g) and 1-hydroxybenzotriazole hydrate (0.201 g). After stirring for 15 min, N-Boc-1,6-diaminohexane (0.322 g) was added. The reaction mixture was allowed to warm to RT and stirred overnight. Solids were filtered off and they were washed with EtOAc. The filtrate and washings were then concentrated under reduced pressure. The resulting residue was purified by flash column chromatography (0 to 10% MeOH in CH2Cl2) to afford Fmoc-Phe-Gly-NH—(CH2)6NH-Boc as a white solid (0.9 g).