6-乙酰氨基己酸

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 6-acetamidohexanoate was prepared as a low-melting solid by sequential treatment of 6-acetamido hexanoic acid with thionyl chloride and methanol. Five grams of this compound, (27 mmol) was dissolved in an excess of 40% aqueous methylamine solution, and the resulting mixture was stirred for sixteen hours at room temperature. The reaction mixture was saturated with sodium chloride and extracted several times with chloroform. The organic layer was dried over magnesium sulfate, and the solvent was removed in vauo to yield a crude residue. Recrystallization from THF yielded 4.5 grams (90%) of pure product, melting point 99°-100° C. extracted several times with chloroform The organic layer was dried over magnesium sulfate the solvent was removed in vauo to yield a crude residue

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Methyl 6-acetamidohexanoate was prepared as a low-melting solid by sequential treatment of 6-acetamido hexanoic acid with thionyl chloride and methanol. Five grams of this compound, (27 mmol) was dissolved in an excess of 40% aqueous methylamine solution, and the resulting mixture was stirred for sixteen hours at room temperature. The reaction mixture was saturated with sodium chloride and extracted several times with chloroform. The organic layer was dried over magnesium sulfate, and the solvent was removed in vauo to yield a crude residue. Recrystallization from THF yielded 4.5 grams (90%) of pure product, melting point 99°-100° C. extracted several times with chloroform The organic layer was dried over magnesium sulfate the solvent was removed in vauo to yield a crude residue

实验步骤: 纯化: 取固体加热溶解后，趁热过滤，然后滤液析晶

实验步骤: 投料: 取固体加热溶解后，趁热过滤，然后滤液析晶

实验步骤: 投料: 加入A2，加入氢氧化钠溶液，RT反应，反应1h，送LCMS，反应完后，反应液降温，然后用盐酸调PH至6-8，浓缩掉甲醇，然后加入THF，降温，用盐酸调PH至1-2，过滤反应液，滤液分相，水相用THF萃取一次，有机相合并浓缩,加入水50℃重结晶

实验步骤: 投料: 准备3个棕色小瓶编号A,B,C,一个25ml单口瓶编号D，前三个小瓶A,B,C分别加入0.2gSM(55-151-o)，A加入氢氧化钠 0.064g，B加入氢氧化钠 0.085g，C加入氢氧化钠 0.107g，ABC分别加入THF 0.45ml，水0.2ml，室温搅拌反应 D加入氢氧化钠0.18g，加入水0.7ml，降温至10℃，将SM(55-155-O)0.7Gg溶于1.4mlTHF 中，将其滴加入D中，滴毕后10℃保温反应 \n投料: ABCD取样LCMS CIM100340-75-5-A-IPC1/CIM100340-75-5-B-IPC1/CIM100340-75-5-C-IPC1/CIM100340-75-5-D-IPC1 17:30 取样LCMS CIM100340-75-5-A-IPC2/CIM100340-75-5-B-IPC2/CIM100340-75-5-C-IPC2/CIM100340-75-5-D-IPC2

实验步骤: 投料: 加入原料，THF，氢氧化钠溶液，然后RT反应\n监测: 送LCMS中控，原料还有剩余 13：45 补加0.5eq的氢氧化钠 8月1日 10:00 补加0.5eq氢氧化钠 11：00 送LCMS中控\n后处理: 反应液有固体析出，过滤反应液，固体（G1）送LCMS（有少量产品），滤液分相得到有机相（O1），水相(W1)，W1用浓盐酸调PH至2-3，有固体析出，过滤得到固体(G2)，滤液，G1加到滤液中（变碱性），继续用浓盐酸调PH至2-3，过滤得到固体(G3)，滤液分相，有机相浓缩，G2和G3用THF打浆，然后过滤，没有得到产品，O1浓缩得到8.1g产品，用24mlEA打浆，过滤，固体加入EtOH浓缩

实验步骤: 投料: 加入原料，氢氧化锂，THF，水，然后RT反应\n监测: LCMS中控

实验步骤: 投料: 加入200mg原料，DBU，乙酸酐1ml，RT反应\n监测: 送LCMS中控

实验步骤: 投料: 取5个小反应瓶，各加入200mg原料，然后A中加入5%碳酸钾溶液，B中加入5%碳酸铯溶液，C中加入5%碳酸钠溶液，D中加入5%氢氧化锂溶液，E中加入5%氢氧化钾溶液\n监测: 送LCMS中控