1172623-99-2 ((2R,3S)-2-(2,5-二氟苯基)-5-羟基四氢-2H-吡喃-3-基)氨基甲酸叔丁酯

作为医药中间体，用于相关药物的合成制备。

医药

合成路线 1（1. 合成：1172623-99-2）

产率：84% 合成条件：Stage #1: With dimethylsulfide borane complex In tetrahydrofuran; tert-butyl methyl ether; toluene at -10 - 0℃; for 3.50 h; Stage #2: With sodium hydroxide In tetrahydrofuran; tert-butyl methyl ether; water; toluene at 20 - 30℃; for 0.25 h; Stage #3: With sodium perborate In tetrahydrofuran; tert-butyl methyl ether; water; toluene at 20 - 30℃; 实验步骤：将1G（8.9g，28.6mmol）溶于无水甲基叔丁基醚（90ml）中，向其中加入无水甲苯（9ml），将温度降至-10℃，并加入硼烷二甲基硫醚的溶液。逐滴加入四氢呋喃（2mol / l，35.9ml），然后在0℃下反应3.5小时。缓慢加入水（4ml），滴加氢氧化钠溶液（1mol / l，89ml），搅拌15分钟，分批加入过硼酸钠（13.2g，85.8mmol），然后搅拌在室温下过夜。使反应溶液沉降并分配，水相用甲基叔丁基醚（50ml32）萃取。合并有机相，用饱和氯化钠溶液（20ml32）洗涤，加入无水硫酸钠干燥，过滤，浓缩，然后加入甲苯（50ml），加热溶解至90℃。将正己烷（200ml）滴加到反应溶液中，沉淀出白色固体，然后过滤。将滤饼用正己烷（30ml32）洗涤，浓缩除去溶剂，得到白色固体粉末1H（7.9g，收率84％）.MS m / z（ESI）：274.1 [M-55] 。 参考文献：

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