87579-78-0 (2S,5R)-3,3-二甲基-7-氧代-4-硫杂-1-氮杂双环[3.2.0]庚烷-2-羧酸二苯甲酯 4-氧化物

运输信息：冰袋运输。危险描述：非危险化学品。

化学合成。

化学合成

路线1：

• 步骤: 向500mL三颈烧瓶中加入250mL四氢呋喃和AT-2湿产物，加入136g 36％乙酸铵水溶液，降温至0-5℃，缓慢加入15g锌粉，保温30分钟后过滤，水相用100mL THF萃取，合并有机相减压浓缩结晶，过滤，50-60℃干燥得成品。
• 条件: With ammonium acetate; zinc In tetrahydrofuran; water at 0 - 10℃;
• 收率: 82.9%（摩尔收率82.1%）
• 参考文献: [1] Patent: CN108264519, 2018, A. Location in patent: Paragraph 0065; 0072; 0073

路线2：

• 步骤: 将82.6g化合物1溶解在300mL二氯甲烷中，加入115mL 20％氯化铵水溶液和36mL甲醇，加入1.6g氯化铋后，逐渐加入10g铝粉，20-30℃反应5小时，加入120mL水，过滤不溶性金属残余物，分离有机层，用120mL 5％氯化钠水溶液洗涤，浓缩得化合物2。
• 条件: With bismuth(III) sulfate; ammonium chloride; aluminium In methanol; dichloromethane; water at 20 - 30℃; for 5 h;
• 收率: 89%（实施例2）
• 参考文献: [1] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [2] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [3] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [4] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [5] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [6] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [7] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [8] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [9] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [10] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [11] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [12] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [13] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [14] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [15] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [16] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 6 [17] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 7 [18] Heterocycles, 1996, vol. 43, # 11, p. 2337 - 2342

路线3：

• 步骤: 向反应烧瓶中加入400mL乙醇，冷却至0-5℃，分三份加入15.2g硼氢化钠（间隔10分钟），加完后0-5℃搅拌30分钟，升温至25℃反应1小时，降温至5-10℃，滴加50mL 1M盐酸，减压浓缩回收乙醇，用乙酸乙酯（100mL×3）萃取，合并有机层，加入乙醇，用50mL水洗涤，浓缩回收乙酸乙酯至约100mL，加入50mL正己烷，冷却至10-15℃得晶体。
• 条件: With sodium tetrahydroborate In ethanol at 0 - 25℃; for 1.50 h;
• 收率: 93.1%（HPLC纯度99.5%）
• 参考文献: [1] Patent: CN108250218, 2018, A. Location in patent: Paragraph 0035-0036; 0038 [2] Patent: EP1666482, 2006, A1. Location in patent: Page/Page column 7