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[求助]
求翻譯一段實驗操作
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10 g of N1A(底物) were dissolved in 1000 ml of water, then 108 g of aluminium trichloride were added. The mixture was heated up to 85° C. then 2 g of Pd/C 5% 50% wet was added to the mixture. The suspension so obtained was then hydrogenated under pressure (500 psi) under vigorous agitation for 36 hrs at a temperature of 85° C. The catalyst was then recovered by filtration maintaining the temperature above 60° C. Then 50 ml of toluene were added and the mixture treated with NaOH 30% (40 ml) till pH12 and clear solution was obtained. The clear aqueous phase, containing sodium aluminium hydroxides was discharged; the toluene solution was washed two times with small quantity of cold water (3 ml) for the sake of removing the un-reacted starting material. The toluene solution was then concentrated under vacuum till residue, the residue was taken up with acetone 40 ml. Hydrochloric acid was bubbled maintaining the mixture temperature below 15° C. to get precipitation of N2A in highly pure form, which was cooled to 5° C. and then collected obtaining 9.0 g of N2A(產物) yield: 98.2%-purity 99.9%. |
銅蟲 (正式寫手)
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10g N1A 溶解在1000ml水中,加入108g 三氯化鋁;旌衔锛訜岬85℃,然后在5%50%濕度下加入2g Pd/C.所得混懸液在壓力(500psi),85°C,劇烈攪拌36h下氫化。 該催化劑在溫度維持在60℃以上過濾回收。然后加入50ml甲苯,并用30%(40ml)NaOH調節(jié)混合物的pH在12,得到澄清的溶液。澄清的水溶液種含有被排除的氫氧化鈉鋁。用少量冷水(3ml)洗滌甲苯溶液兩次,除去未反應的原料。然后再真空下濃縮甲苯溶液至殘余物,殘余物溶于40ml丙酮中。在15℃下向混合物種鼓入鹽酸,得到高純度的N2A沉淀,將其冷卻至5℃,然后收集9.0g N2A,收益率:98.2%,純度99.9%。 |

銀蟲 (正式寫手)
銀蟲 (正式寫手)
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將10克的底物溶解于1000毫升的水中得溶液A,再將108克的三氯化鋁加入上述溶液A得到混懸物B,將所得的混懸物B加熱至85度。然后繼續(xù)加入2克鈀碳(鈀碳的規(guī)格為5%,50%濕度)得到混懸物C。將上述混懸物C置于催化氫化反應釜(壓力為500psi,溫度為85度)劇烈攪拌震蕩36小時。 將催化劑(即鈀碳)趁熱(溫度維持在60度以上)過濾除去。濾液保留并加入50毫升的甲苯得到溶液D。向溶液D中緩慢滴加30%的氫氧化鈉(約40毫升)直到PH值變?yōu)?2,此時得到溶液E。溶液E是含有有機層和水層亮相的溶液,用分液漏斗除去水層(即下層),保留有機層(即甲苯層)。有機層用冷水洗兩次,然后減壓蒸去甲苯得物質F。將物質F溶于40毫升丙酮,然后在15度以下的溫度持續(xù)通氯化氫氣體得到沉淀即物質F的鹽酸鹽。繼續(xù)冷卻至5度是的沉淀完全析出。收集沉淀物即上述鹽酸鹽得最終產物。 |

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