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4-Methoxy-4-oxobutanoic acid (1) Succinic anhydride {40.0 g) was added to a well stirred solution of methanol anhydride (25.0 mL) at 20--25℃. The reaction mixture was heated at 100-1100C for 3 h, cooled to room temperature and then concentrated at reduced pressure to give product 1 (50.2 g, 95%). The crude product was practically pure, and used for the next step without further purification. An analytical sample was obtained by recrystallization from EtOH/Hexane. Methyl 4-cyano-4-oxobutanoate (2) A stirred mixture of compound 1 (8.8 g) was chlorinated by the addition of thionyl chloride (10 mL) under NZ gas at 35 0C for 5 h. The resulting reaction mixture was concen-trated at reduced pressure, yielding the crude product, to which was then added a stirred solution of CuCN (5.5 g) in acetonitrile (20 mL). The reaction mixture was heated at 700C for 8 h, cooled to room temperature and then filtered through celite, and the organic solution then con-centrated at reduced pressure to yield the desired product 2 (6.4 g, 68%). 5-Aminolevulinic acid hydrochloride (3) A stirred mixture of compound 2 (5.4 g) was hydro-genated by the addition of Pd/C (0.5 g) in 6M HCI under apressure of 125 psi at room temperature for 18 h. The re- suiting mixture was filtered through celite, and the organicsolution concentrated at reduced pressure, yielding thecrude product. The crude product was purified, by recry-stallization with EtOH/2-propanol, to yield the pure product3 as a solid (5.7 g, 89%). t -Butyl 5-aminolevulinate (4) Compound 3 (1.6 g) was dissolved in water at room temperature一this solution was added 2M NaOH until apH 7 was obtained, and the whole mixture was then extracted with Et2O (3*10 mL), dried over MgS04, and concentrated at reduced pressure to yield the crude product. A stirred mixture of the crude product, 2-methylpropene and H2S04 (0.1 mL) in Et20 (10 mL). The reaction mixture was stirred at room temperature for 10 h, with its subsequent addition to 2M HCI (1.5 mL). After 2 h, the reaction mixture was concentrated at reduced pressure. The crude product was purified by recrystallization from EtOH to yield the pure product 4 as a solid (1.3 g, 58%) RESULTS AND DISCUSSION Cancer is a very serious health problem, with early therapy offering the only chance of a cure. Apart from non-invasive screening methods there is also the need for better bronchoscopic techniques. 5-minolevulinic acid can be applied for the simple diagnosis of cancer. Therefore, a simple method for the synthesis of 5-ALA, using cheap starting materials and a very simple refining process, has been developed in our laboratory. The induced fluorescence of this compound is useful in the planning of photodynamic therapy and diagnosis. |
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zhaoshans
铁杆木虫 (小有名气)
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风轻轻吹(金币+20,VIP+0): 6-6 12:34
风轻轻吹(金币+20,VIP+0): 6-6 12:34
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4-甲氧基-4-氧桥丁酸 在20-25℃，将40g琥珀酸酐加入到充分搅拌的25mL甲醇酐溶液中，将反应混和物在100-1100C加热3h，冷却到室温，减压下浓缩得到产品1（50.2g，95%）。这种粗产品几乎是纯的，下步应用中不需要后续的纯化。通过乙醇/正己烷重结晶得到分析样品。 甲基4-氰基-4-氧桥丁酸 向8.8g化合物1加入10mL亚硫酰二氯，在NZ气体下350度搅拌5h，使化合物1氯化。此合成混合物在减压条件下浓缩，得到粗产品。向此产品中加入CuCN的乙腈溶液（5.5gCuCN溶解在20mL乙腈中），将反应混合物在700度下加热8h，冷却至室温，经过硅藻土过滤，得到的有机溶液减压浓缩得到需要的产物2（6.4g，68％） 5-氨基酮戊酸氢氯化物 将0.5gPd/C加入到6M HCl中，将上述混合物加入到5.4g化合物2中，然后在125 psi压力、室温条件下搅拌18h，使化合物2氢化。此反应混合物经过硅藻土过滤，得到的有机溶液减压浓缩得到粗产物。粗产物经过纯化，乙醇、异丙醇重结晶，得到纯的固体产物3（5.7g，89%） [ Last edited by zhaoshans on 2009-6-6 at 11:27 ] |
2楼2009-06-06 11:12:50
zhaoshans
铁杆木虫 (小有名气)
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t-丁基－5-氨基铜戊酸盐 1.6g化合物3室温下溶解在水中，向溶液中加入2M NaOH直到pH为7，得到的混合物用乙醚萃取（分三次，每次10mL），用MgSO4干燥，减压浓缩得到粗产物。将此粗产物、2-甲基丙烯和0.1mLH2SO4加入到10mL乙醚中，室温下搅拌10h，随后加入1.5mL 2M HCl。继续搅拌2h后，减压浓缩。粗产物经过乙醇重结晶纯化，得到纯的固体产物4（1.3g，58%） 结果与讨论 癌症作为一种很严重的健康问题，早期的治疗方法很少能治愈。除了无创性方法外，还需要更好的支气管镜的工艺。5-minolevulinic酸可以应用于简单的癌症诊断。因此，我们实验室开发了一种用廉价原料和简单提炼工艺合成5-ALA的方法。这种化合物具有荧光感应性，可以用于癌症的光动力学治疗和诊断 [ Last edited by zhaoshans on 2009-6-6 at 11:28 ] |
3楼2009-06-06 11:26:02
zhaoshans
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4楼2009-06-06 11:27:03