1、将500L搪瓷釜抽真空到60oC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.2Charging/投料Order/顺序向瓶中加入A 10ml(1mol),B (2 g, 2mol) and 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
2、 (10 g, 1 mol) and E (20 ml) were added in turn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 into a solution (mixture or suspension) ofA (10 ml, 1 mol) and B (2 g, mol) in C (50 ml) in turnWay/方式氮气保护下,控温2030oC,通过固体加料漏斗一次性向100L
3、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 while maintaining the temperature at 2030oC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510minA(10.0kg, 10.0mol) was ad
4、ded to a 500L stainless steel reactor in four portions (2.5kg4) at interval of 510min while maintaining the temperature at 2030oC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2030
5、oC, 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
6、) by nitrogen at 2030oC and then the stirrer 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
7、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。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 B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
8、 mole, 2.5 M in hexane) was added into asolution of A in solvent B via cannula, dropping funnel or syringe over a period of 5h3Add dropwise滴加控温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
9、 or constant pressure funnel) at a rate of 1520kg/h while maintaining the temperature at 1015oC.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 maintaining gentl
10、e reflux; while keeping inner temperature between 10oC 30oC) under nitrogen4Heat升温将体系升温至1520oC,升温速度510oC/hThe mixture was heated to 1520oC at the rate of 510oC/h.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.5Cool降温将体系降温至1520oC,降温速度510/hThe mixture was cooled
11、to 1520oC at the rate of 510oC/h.用外浴乙醇/液氮将体系降温至-70-75oCThe mixture was cooled to -70-75oC by ethanol/liquid nitrogen6Maintain保温将体系于1520oC保温搅拌0.5h。The mixture was stirred at 1520oC for 0.5h。7Reflux回流体系于7882oC回流3h。The mixture was refluxed at 7882oC for 3h.8Exchange/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0.2
12、MPa,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 nitrogen and pumped down to normal pressure each time. And then the mixture was exchanged with hydrogen under liquid level for 5
13、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 2030oC9React反应Type/类型无溶剂反应: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
14、in solvent C, evaporated to dryness and heated at 50oC for 2h。催化量的反应:于0oC,加入A (20 ml, 142 mmol)和催化量B(1微量或两滴),加入C(4.549 g, 46.4 mmol)的D (120ml)溶液中。A (20 ml, 142 mmol) and catalytic amount (a trace amount or two drops) of B were added into a solution of C (4.549 g, 46.4 mmol) in D (120mL) at 0oC闷罐反应或封
15、管反应:控温T=40oC,P=0.5MP ,A(1g, 1mol)的饱和氨水(或其他气体如:一氧化碳、二氧化碳、硫化氢)乙醇(1ml)溶液在50ml封管或闷罐/高压釜中搅拌5小时。A solution of A (1g, 1mol) in ethanol (x ml) saturated with NH3 (or other gas such as: CO,CO2, H2S) was stirred under 0.5MPa at 40oC for 5hrs in a 50 ml of sealed tube or autoclave.A(1g, 1mol) 的饱和氯化氢甲醇(1ml) 溶液在
16、20oC搅拌。A solution of A (1g, 1mol) in methanol (1ml) saturated with HCl was stirred at 20oC.控温20oC,向A(1g, 1mol)的甲醇(1ml)溶液中通臭氧15min。然后通氮气除臭氧,再于20oC加入Me2S (5ml)。Ozone was bubbled into a solution of A (1g, 1mol) in MeOH (1ml) at 20oC for 15minutes. After excess O3 was purged by N2, Me2S (5ml) was added
17、at 20oC.A(1g, 1mol)和B(1g, 1mol)的C(1ml)溶液在30oC下通气体0.5小时。Gas was bubbled into a solution of A (1g, 1mol) and B (1g, 1mol) in solvent C (1ml) at 30oC for 0.5h.控温10oC,D(1g, 1mol) 加入到A(1g, 1mol)的B(5ml)和C(10ml)溶剂混合液(或B和C的混合溶剂)中,反应体系搅拌(回流或加热)两小时。To a solution of A (1g, 1mol) in a mixture of solvent B (5ml)
18、 and solvent C (10ml) (or a mixed solvent of B and C) was added D (1g, 1mol) at 10oC, the reaction mixture was allowed to stir (reflux or heat) for 2h.向A(1g, 1mol)的丙酮水溶液(丙酮:水=10:1)中加入B (1g, 1mol),再加入C(1g, 1mol),反应体系搅拌(回流或加热)五小时。To a solution of A (1g, 1mol) in 10: 1 aqueous acetone (1ml) was added B
19、 (1g, 1mol) followed by addition of C (1g, 1mol), the reaction mixture was allowed to stir (reflux or heat) for 5hrs.将A和B溶于苯或甲苯,体系回流1h,共沸带水。A (x g, x mol) and B (x g, x mol) in benzene or toluene (x mL) were refluxed for xh with azeotropical removal of water.将A、B和甲苯磺酸的甲苯溶液加热回流,用分水器除水。A mixture of A,
20、 B and TsOH.H2O (56.91 g, 0.3 mol) in toluene (400 mL) was heated toreflux and remove water by Dean-Stark trap.氮气保护下,向A的乙醇溶液中加入Pd-C或Ra-Ni或Pd(OH)2/C。悬浮液真空下除氧,再通几次氢气。To a solution of A (x g, x mol) in EtOH (x mL) was added Pd-C or Ra-Ni or Pd(OH)2/C (10%,x g) under N2. The suspension was degassed unde
21、r vacuum and purged with H2 several times.体系于5 psi ,20oC搅拌氢化1h。氢化瓶或高压釜The mixture was stirred under H2 (5 psi) at 20oC for 1h. 体系于20oC搅拌氢化1h。常压氢化如气球反应The mixture was stirred under H2 balloon at 20oC for 1h.A和Ra-Ni的乙醇溶液在室温、50Psi氢气压力下氢化2h。A mixture of A (x g, x mol) and Ra-Ni (x g) in EtOH (x ml) was
22、hydrogenated under50 Psi of hydrogen pressure for 2h at room temperature.Condition or process/条件或过程反应体系(溶液或悬浮液)于5oC搅拌2hrs后,于室温保温2hrs(或过夜)。The reaction mixture (solution or suspension) was stirred at 5oC for 2h and then kept at room temperature (or ambient temperature) for another 2h (or overnight)反应
23、体系(溶液或悬浮液)于60oC回流2hrs(或过夜)。The reaction mixture (solution or suspension) was refluxed at 60oC for 2h (or overnight)反应体系(溶液或悬浮液)容许回流2hrs(或过夜)。The reaction mixture (solution or suspension) was allowed to reflux (or heat to reflux) for 2h (or overnight)反应体系(溶液或悬浮液)容许回温2hrs后, 回流2hrs(或过夜)The reaction mix
24、ture (solution or suspension) was allowed to warm to temperature during 2h and reflux for 2h (or overnight)State or Endpoint of reaction/反应状态或终点反应通过TLC(石油醚:乙酸乙酯=4:1),LC-MS,液相或核磁确认完成(为完成或杂乱的)。The reaction was complete (incomplete or messy) detected (determined or confirmed) by TLC (PE/EtOAc 4:1), LC-
25、MS, HPLC or NMRTLC(石油醚:乙酸乙酯=1:1)或液相(107757-088-1)显示反应结束。TLC (PE:EtOAc=1:1) or HPLC (107757-088-1) showed or indicated that the reaction was complete.1)或液相(107757-088-1)显示起始原料完全消耗。1) or HPLC (107757-088-1) showed the starting material was consumed completely.1)或液相(107757-088-1)显示根本没有反应或大部分原料剩余。 EtOAc
26、 =1:1) or HPLC (107757-088-1) showed the reaction didnt work at all or most of starting material was still remained.起始原料完全消耗,但经MS (106657-078-1) 或LC-MS (106657-078-1)检测,没有预期的产物。The starting material was consumed completely, but no desired compound was detected or determined by MS (106657-078-1) or L
27、C-MS (106657-078-1).TLC显示有几个点Several spots were shown on TLC.经MS (106657-078-1) 或LC-MS (106657-078-1)或 HPLC (106657-078-1) 或TLC (石油醚:1).检测,只有很少量的预期产物。Only a trace amount of desired compound was detected by MS (106657-078-1) orLC-MS (106657-078-1) or HPLC (106657-078-1) or TLC (PE:1).由于收率低或溶解性不好,通过层析
28、或制备的高效液相色谱仪,不能分离或纯化预期化合物,。The desired compound could not be isolated, separated or purified by chromatography or prep. HPLC due to poor yield or poor solubility.通过1H NMR (106675-010-2) or MS确认,得到(或分离)的不是预期化合物,反应失败。1H NMR (106675-010-2) or MS confirmed the obtained (or isolated) compound is not the desired compound. The reaction failed.Scaling up technic in Asymchem/放大工艺中体系
copyright@ 2008-2022 冰豆网网站版权所有
经营许可证编号:鄂ICP备2022015515号-1