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1、1 of 14STANDARDIZED PHRASE FOR REPORT/英文报告标准用语 Process Description/工艺描述No. Unit Operations Process description in Chinese Process description in English装有机械搅拌( 或磁力搅拌)，加料漏斗，温度计(或分水器，干燥管) 的 3L 三口瓶A 3L three-necked round bottom flask equipped with mechanical stirrer (or magneticstirrer), addition funne
2、l and thermometer (or Dean-Stock; drying tube)反应中所用的所有瓶子，真空条件下加热 30min，氮气吹扫 10min。All flasks used in the reaction were heated under vacuum for 30 minutes and purged with nitrogen for 10 minutes.将 500L 高压釜通氮气至 0.40.5MPa。若 0.51h内压力无变化，则气密性良好。A 500L autoclave reactor was filled with nitrogen to increas
3、e the pressure to 0.40.5MPa. If the pressure had no change within 0.51h, then the air-tightness of the autoclave reactor was good.将 500L 搪瓷釜抽真空到60 oC 用氮气烘 68h，然后降温到 2025oC。A 1000L titanium reactor was dried at 60oCwith hot nitrogen for 68h, then cooled to 2025oC.向瓶中加入 A 10ml(1mol)，B (2 g, 2mol) and
4、C (50 ml ) The flask was charged with A (10 ml, 1 mol), B (2 g, 2mol) and C (50 ml )依次加入 D (10 g, 1 mol) and E (20 ml) D (10 g, 1 mol) and E (20 ml) were added in turnOrder/顺序 向 A(10ml, 1 mol)和 B (2 g, mol)的 C(50ml)溶液(体系 或悬浮液)中，依次加入 D (10 g, 1 mol) 和 E (20 ml)D (10 g, 1 mol) and E (20 ml) were added
5、 into a solution (mixture or suspension) ofA (10 ml, 1 mol) and B (2 g, mol) in C (50 ml) in turn氮气保护下，控温 2030oC，通过固体加料漏斗一次性向 100L 搪瓷釜中加入 A (40.0kg, 10.0mol)Under the protection of nitrogen, A(40.0kg, 10.0mol) was added into a 100L glass-lined reactor in one portion via the solid additional funnel w
6、hile maintaining the temperature at 2030oC2 Charging/投料Way/方式 控温 2030oC， 向 500L 白钢釜中， 分四批加入 A (10.0kg, 10.0mol)，每批 2.5kg，间隔时间为A(10.0kg, 10.0mol) was added to a 500L stainless steel reactor in four portions (2.5kg4) at interval of 510min while maintaining the temperature at 2030oC2 of 14No. Unit Oper
7、ations Process description in Chinese Process description in English510min将 D (10 g, 1 mol) 分批加入， 1h 加完。 D (10 g, 1 mol) was added in portions during a period of 1 h.将 D (10 g, 1 mol) 分批加入， 1h 内加完。 D (10 g, 1 mol) was added in portions within 1 h.控温 2030oC， 用真空向干燥洁净的 100L 搪瓷釜中抽入 114260 的乙酸乙酯溶液( 外标折算
8、后为50.0kg 114260)。Maintaining the temperature at 2030oC, solution of 114260 in ethyl acetate (50.0kg 114260 corrected by wt%) was added by vacuum to a clean and dried 100L glass-lined reactor控温 2030oC，用氮气压入 A(100kg, 101mol)，开动搅拌，A(100kg,101mol) was added(charged) by nitrogen at 2030oC and then the st
9、irrer was started.控温 2030oC，用真空抽入 A(100kg, 101mol) Maintaining the temperature at 2030oC, A (100kg,101mol) was added(charged) by vacuum.控温 2030oC，用泵打入 A(100kg, 101mol) A(100kg,101mol) was added(charged) by pump while maintaining the temperature at 2030oC将正丁基锂或硼烷/四氢呋喃溶液(10 ml, 1 mole, 2.5 M in 己烷) ，通
10、过管路导入滴加漏斗或 A 的 B 溶液中。A solution of BuLi or BH3/THF (10 ml, 1 mole, 2.5 M in hexane) was cannulated intoaddition funnel or into a solution A in solvent B2 Charging/投料 Way/方式通过插管，滴加漏斗或针筒，将正丁基锂或硼烷/四氢呋喃溶液(10 ml, 1 mole, 2.5 M in 己烷) ，通过管路导入滴加漏斗或 A 的 B 溶液中， 5h 加完。A solution of BuLi or BH3/THF (10 ml, 1 m
11、ole, 2.5 M in hexane) was added into asolution of A in solvent B via cannula, dropping funnel or syringe over a period of 5h控温 1015oC，通过 50L 滴加罐( 高位瓶或恒滴)向体系中滴加 D (101kg, 10 mol)，滴速为1520kg/h。D (101g, 10mol) was added dropwise into the mixture through (via) 50L additional vessel (or carboy or constant
12、 pressure funnel) at a rate of 1520kg/h while maintaining the temperature at 1015oC.3 Add dropwise滴加 控温 10oC(或保持微回流或保持内温 1030oC)，氮气保护下，(通过加料漏斗或针筒)滴加 D (10 g, 1 mol) 的 E (20 ml)溶液。a solution of D (10 g, 1 mol) in E (20 ml) was added dropwise (via addition funnelor syringe) at 10oC (or while maintaini
13、ng gentle reflux; while keeping inner temperature between 10oC 30oC) under nitrogen将体系升温至 1520oC，升温速度 510oC/h The mixture was heated to 1520oC at the rate of 510oC/h.4 Heat升温 用汽水混合器将体系升温至 5060oC。 The mixture was heated to 5060oC by the steam-water mixing heating.3 of 14No. Unit Operations Process de
14、scription in Chinese Process description in English将体系降温至 1520oC，降温速度 510/h The mixture was cooled to 1520oC at the rate of 510oC/h.5 Cool降温 用外浴乙醇/液氮将体系降温至-70-75 oC The mixture was cooled to -70-75oC by ethanol/liquid nitrogen6 Maintain保温 将体系于 1520oC 保温搅拌 0.5h。 The mixture was stirred at 1520oC for
15、0.5h。7 Reflux回流 体系于 7882oC 回流 3h。 The mixture was refluxed at 7882oC for 3h.8 Exchange/置换控温 2030oC，将氮气通入液面下置换体系 10 次，每次通氮气至 0.2MPa，然后排空至常压；再液面下通氢气置换体系 5 次，每次通氢气至 0.2MPa，然后排空至常压。（高压反应中用到）The mixture was exchanged with nitrogen under liquid level for 10 times. The pressure was increased to 0.2MPa with
16、 nitrogen and pumped down to normal pressure each time. And then the mixture was exchanged with hydrogen under liquid level for 5 times. The pressure was increased to 0.2MPa with hydrogen and pumped down to normal pressure each time. During exchanging, the temperature of mixture was controlled at 2030oC无溶剂反应：将 A (1 g, 1 mol) and B (1 g, 1 mol)溶于溶剂 C 中，蒸干后，于 50oC 加热 2 小时。A (1 g, 1 mol) and B (1 g, 1 mol) were dissolved in solvent C, ev
