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[求助]
求高手翻译一段有机合成步骤
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求高手翻译一段有机合成步骤,一定要通顺啊。这个步骤对我的实验非常重要。 N-(3-Chloro-2-nitrophenyl)glycine (12). 3-Chloro-2-nitroaniline (5.12 g, 29.7 mmol) was heated with bromoacetic acid (4.25 g, 29.7 mmol) at 125 °C for 1 h with air passing over the mixture to remove the HBr. Methanol was then added and the mixture heated until all the solid dissolved. Dilute NH4OH was added in portions to maintain the pH > 8 while the mixture was concentrated by heating. The cooled mixture was filtered and then washed with dilute NH4OH, and the filtrate was washed with ether (50 mL). The aqueous layer was then concentrated to a small volume and acidified while hot to pH 3 with concentrated HCl. After cooling, the product was collected, washed with ice-water, and dried to give 12 as a yellow-brown solid: mp 195-197 °C (dec). Additional product was obtained by extracting the filtrate with AcOEt (2 *25 mL) and washing the extracts with saturated NaCl (25 mL). After the extract was dried (MgSO4), it was concentrated togive a yellow solid (total 0.42 g, 6% total yield)。 |
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chillgame111
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【答案】应助回帖
★
Mally89: 金币+1, 感谢应助,欢迎常来哈! 2012-06-21 19:57:50
Mally89: 金币+1, 感谢应助,欢迎常来哈! 2012-06-21 19:57:50
| N-(3-氯-2-硝基苯基)甘氨酸. 3-氯-2-硝基苯胺(5.12 g, 29.7 mmol)和溴乙酸(4.25 g, 29.7 mmol)在125℃的条件下,加热1小时后,向体系中鼓入空气除掉生成的溴化氢气体,向体系中加入甲醇,加热的条件下,至固体溶解。分批加入稀释的氨水维持pH大于8,接着体系在加热条件下浓缩。浓缩完得体系冷却后过滤,滤液依次用稀释的氨水和乙醚(50mL)洗涤。水相浓缩至小体积后,趁热用浓盐酸调节pH等于3。冷却,收集产品,产品用冰水洗涤,干燥得灰褐色固体:熔点195-197℃,另外通过用乙酸乙酯(2 *25 mL) 萃取母液,饱和氯化钠溶液(25 mL)洗涤萃取液,硫酸镁干燥萃取液,后浓缩得到黄色的产品。(总共0.42g,总收率6%) |
2楼2012-06-20 14:13:47
yangxiuhuaya
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3楼2012-06-29 15:28:53











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