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[求助]
求幫忙翻一個實驗操作,萬分感謝
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| The solution obtained in example 2), containing 45 g of NA1-hydrochloride together with 53.3 g of aluminium tri-chloride and 10.7 g of ammonium chloride, was heated up to 65.deg. C. under hydrogen together with 1 g of Pd/C 5percent 50percent wet. The suspension so obtained was then hydrogenated under pressure (50 psi) under vigorous agitation for 6 hrs then the temperature was risen up to 85.deg. C. and the hydrogenation was prolonged for 36 hrs, at a temperature of 85.deg. C.During the reaction time further 4 g of Pd/C 5percent 50percent wet were added to the mixture.The catalyst was then recovered by filtration maintaining the temperature above 60.deg. C. Then 250 ml of toluene were added and the mixture treated with NaOH 30percent (200 ml) till pH12 and clear solution was obtained. The clear aqueous phase, containing sodium aluminium hydroxides was discharged; the toluene solution was washed twice with small quantity of cold water (15 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 200 ml. Hydrochloric acid was bubbled maintaining the mixture temperature below 15.deg. C. to get precipitation of NA2-hydrochloride in highly pure form, which was cooled to 5.deg. C. and then collected obtaining 41.8 g of NA2-hydrochloride yield (two steps): 90.2percent purity 99.4percent. |
銅蟲 (正式寫手)
| 樣品2中得到的溶液,含45克NA1-鹽酸與53.3克三氯化鋁以及10.7克氯化銨,在氫氣條件下與1克的Pd / C 5%,50%濕度,一起加熱到65攝氏度。這樣得到的懸浮液,然后在壓力( 50 psi)下劇烈攪拌氫化6小時,然后將溫度上升至85攝氏度,并在該溫度下氫化延長至36小時。在反應期間,進一步加入4克的Pd / C 5%,50%濕度至混合物中,然后過濾回收,保持溫度在60攝氏度以上。然后加入250毫升甲苯并用30%NaOH (200毫升),調混合物至PH12 ,獲得澄清的溶液。澄清的水相,含有氫氧化鋁鈉被排出,為了除去未反應的起始原料,用含有少量的冷水(15毫升)的甲苯溶液洗滌兩次。該甲苯溶液,在真空下濃縮至殘余物,殘余物溶于200毫升的丙酮中。保持混合物溫度低于15攝氏度并吹入鹽酸。 冷卻到5攝氏度,得到高純度的NA2-鹽酸沉淀形式,然后收集得到41.8克NA2-鹽酸鹽的產率(兩個步驟) :純度為 90.2%和99.4% 。 |

木蟲之王 (文壇精英)
童心看世界!
| 實施例2中得到的溶液,含45克NA1-鹽酸與鋁三氯化53.3克以及10.7克氯化銨一起被加熱到65攝氏度,在氫氣條件下與1克的Pd / C 5%,50%濕度一起。這樣得到的懸浮液,然后在劇烈攪拌下( 50 psi)的壓力下氫化6小時,然后將溫度上升至85攝氏度,在溫度85攝氏度下氫化延長了36個小時。進一步加入4克的混合物.催化劑的Pd / C 5%,50%濕度,然后通過過濾回收,保持溫度高于60攝氏度。然后加入250毫升甲苯中加入,并處理該混合物至PH12 ,獲得澄清的溶液,用NaOH (200毫升) 30percent 。清晰的水相,含有鋁鈉的氫氧化物被排出,為了除去未反應的起始原料,用少量的冷水(15毫升)的甲苯溶液洗滌兩次。的甲苯溶液,然后在真空下濃縮至殘余物,殘余物溶于用丙酮200毫升。保持混合物溫度低于15攝氏度鹽酸鼓泡。 冷卻到5攝氏度,得到高純度的NA2-鹽酸沉淀形式,然后收集得到41.8克NA2-鹽酸鹽的產率(兩個步驟) : 90.2%純度99.4%純度 。 |

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