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qulihua新蟲 (小有名氣)
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[求助]
求高手翻譯一段有機(jī)合成步驟
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求高手翻譯一段有機(jī)合成步驟，一定要通順啊。這個步驟對我的實驗非常重要。 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
木蟲 (小有名氣)
- 應(yīng)助: 1 (幼兒園)
- 金幣: 1575.2
- 紅花: 3
- 帖子: 229
- 在線: 157.5小時
- 蟲號: 533457
- 注冊: 2008-03-26
- 專業(yè): 有機(jī)合成
【答案】應(yīng)助回帖
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Mally89: 金幣+1, 感謝應(yīng)助，歡迎常來哈！ 2012-06-21 19:57:50
Mally89: 金幣+1, 感謝應(yīng)助，歡迎常來哈！ 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℃的條件下，加熱1小時后，向體系中鼓入空氣除掉生成的溴化氫氣體，向體系中加入甲醇，加熱的條件下，至固體溶解。分批加入稀釋的氨水維持pH大于8，接著體系在加熱條件下濃縮。濃縮完得體系冷卻后過濾，濾液依次用稀釋的氨水和乙醚（50mL）洗滌。水相濃縮至小體積后，趁熱用濃鹽酸調(diào)節(jié)pH等于3。冷卻，收集產(chǎn)品，產(chǎn)品用冰水洗滌，干燥得灰褐色固體：熔點195-197℃，另外通過用乙酸乙酯(2 *25 mL) 萃取母液，飽和氯化鈉溶液(25 mL)洗滌萃取液，硫酸鎂干燥萃取液，后濃縮得到黃色的產(chǎn)品。（總共0.42g，總收率6%） |
2樓2012-06-20 14:13:47
yangxiuhuaya
銅蟲 (小有名氣)
- 翻譯EPI: 8
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- 蟲號: 1545573
- 注冊: 2011-12-21
- 性別: GG
- 專業(yè): 微生物生理與生物化學(xué)
【答案】應(yīng)助回帖
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qulihua: 金幣+10, 翻譯EPI+1, ★★★★★最佳答案 2012-07-01 08:20:03
qulihua: 金幣+10, 翻譯EPI+1, ★★★★★最佳答案 2012-07-01 08:20:03
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