三氯氧磷（cas：10025-87-3）是合成实验室经常用使用的化学试剂，广泛应用于有机合成和无机合成中，尤其是在制备磷酸酯、有机磷化合物和某些类型的催化剂时。三氯氧磷是一种强路易斯酸，能够与水反应生成磷酸和氯化氢。在实验室和工业中使用三氯氧磷时需要格外小心，因为它具有腐蚀性，并且对人体有毒性。那么它在缩合反应中表现如何，我们来看看检索结果： 可以看出对硝基苯胺与多种氨基酸都能顺利缩合，产率都普遍较高。通过文献追踪，我们发现其它更多的Boc保护氨基酸反应也能顺利反应，产率非常不错。（pNA=对硝基苯胺） 实验操作：General method：A protected amino acid (10 mmol) and p-nitroaniline (1.38 g, 10 mmol) were dissolved in dry pyridine (30 mL). The clear yellowish solution was cooled to -15℃ and phosphorus oxychloride (1.00 mL, 11 mmol) was added dropwise with vigorous stirring. During the addition the reaction mixture coloured deeply red and became turbid in the course of 5 to 20 min. The colour of the suspension slowly changed to orange, the reaction being complete after a total of 10 to 30 min (monitored by TLC). The reaction mixture was then quenched with crushed ice/water (100 mL) and the nitroanilide was extracted into EtOAc (once 50 mL and three times 30 mL). The combined EtOAc layers were washed with saturated NaHCO3 and NaCl (three times 30 mL each). After drying on Na2SO4 (except the arginine derivatives!). the EtOAc layer was filtered and evaporated in vacuo. The residue was coevaporated successively with toluene, EtOAc and MeOH.
