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tosn铁杆木虫 (职业作家)
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[求助]
求助翻译一段英语
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2楼2013-05-29 23:10:01
tosn
铁杆木虫 (职业作家)
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- 虫号: 392642
- 注册: 2007-06-05
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- 专业: 有机合成
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General procedure for the reductive alkylation of methylamine A mixture of the carbonyl compound (10 mmol), titanium(IV) isopropoxide (5.9 cm3, 20 mmol), methylamine hydrochloride (1.35 g, 20 mmol) and triethylamine (2.79 cm3, 20 mmol) in absolute ethanol (15 cm3) was stirred under Ar at ambient temperature for 8–10 h. Sodium borohydride (0.57 g, 15 mmol) was then added and the resulting mixture was stirred for an additional 7–8 h at ambient temperature. The reaction was then quenched by pouring into aqueous ammonia (2 mol dm23, 30 cm3), the resulting inorganic precipitate was filtered off, and washed with dichloromethane (50 cm3). The organic layer was separated and the remaining aqueous layer was extracted once with dichloromethane (50 cm3). The combined organic extracts were next extracted once with hydrochloric acid (1 mol dm23, 25 cm3) to separate the neutral materials. The acidic aqueous extracts were washed once with dichloromethane (50 cm3), then treated with aqueous sodium hydroxide (2 mol dm23) to pH 10–12, and extracted with dichloromethane (50 cm3 × 3). The combined organic extracts were washed with brine (50 cm3), dried (Na2CO3) and concentrated in vacuo to afford N-methyl secondary amines in good to excellent yield. |
3楼2013-05-29 23:29:40
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tosn: 金币+30, 翻译EPI+1, ★★★★★最佳答案 2013-05-30 18:00:46
tosn: 金币+30, 翻译EPI+1, ★★★★★最佳答案 2013-05-30 18:00:46
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将羰基化合物（10 mmol）、钛（IV）异丙氧化物（5.9cm3,20 mmol），盐酸甲胺（1.35g,20 mmol）和三乙胺（2.79cm3,20 mmol）溶于无水乙醇（15cm3）中，氩气下室温搅拌8-10h。加入硼氢化钠（0.57g,15 mmol），将所得混合物室温下继续搅拌7-8h。倒入氨水（2 mol dm-3,30cm3）使反应猝熄，滤去所得物中的无机沉淀，用二氯甲烷（50 cm3）洗涤。分离有机层，余下水层用二氯甲烷（50 cm3）提取一次。 接下来，将合并后的有机提取物用盐酸(1 mol dm-3,25 cm3)提取一次，以分离中性物质。 酸性水提取物使用二氯甲烷（50 cm3）洗涤一次，再使用氢氧化钠溶液(2 mol dm-3）调节pH到10-12，用二氯甲烷(50 cm3 × 3)提取。合并的有机提取物用盐水(50 cm3)洗涤，干燥(Na2CO3)，真空浓缩以得到高产率的N-甲基二胺。 |
4楼2013-05-30 16:41:07
