| 查看: 890 | 回复: 7 | ||
| 本帖产生 1 个 博学EPI ，点击这里进行查看 | ||
| 当前只显示满足指定条件的回帖，点击这里查看本话题的所有回帖 | ||
whb265金虫 (小有名气)
|
[求助]
求助Boc亚胺的合成方法
|
|
求助Boc亚胺的合成方法 |
回复此楼» 猜你喜欢
全日制（定向）博士
已经有5人回复
-
假如你的研究生提出不合理要求
已经有10人回复
-
萌生出自己或许不适合搞科研的想法，现在跑or等等看？
已经有4人回复
-
Materials Today Chemistry审稿周期
已经有4人回复
-
参与限项
已经有3人回复
-
实验室接单子
已经有4人回复
-
对氯苯硼酸纯化
已经有3人回复
-
求助:我三月中下旬出站，青基依托单位怎么办？
已经有12人回复
-
所感
已经有4人回复
-
要不要辞职读博？
已经有7人回复
121918051
至尊木虫 (著名写手)
- 博学EPI: 12
- 应助: 1 (幼儿园)
- 金币: 10941.1
- 散金: 30
- 红花: 17
- 帖子: 2764
- 在线: 634.8小时
- 虫号: 999319
- 注册: 2010-04-17
- 专业: 有机合成
3楼2010-10-27 09:29:56
whb265
金虫 (小有名气)
- 应助: 0 (幼儿园)
- 金币: 2.8
- 散金: 5
- 帖子: 221
- 在线: 124.3小时
- 虫号: 637859
- 注册: 2008-10-27
- 专业: 高分子物理与高分子物理化
2楼2010-10-26 18:42:01
寒月龙飞
木虫 (小有名气)
- 应助: 0 (幼儿园)
- 金币: 1789.1
- 帖子: 214
- 在线: 105小时
- 虫号: 346841
- 注册: 2007-04-15
- 性别: GG
- 专业: 化学生物学与生物有机化学
【答案】应助回帖
|
两步做：先合成氨基亚砜类化合物，第二部用碳酸钾催化脱去亚磺酸集团。一 A 500-mL flask was charged with tert-butyl carbamate (10.0 g, 85.5 mmol, 1.00 equiv) and benzenesulfinic acid sodium salt (28 g, 170 mmol, 2.0 equiv). Solids were suspended in a solution of methanol in water (1:2, 250 mL). Benzaldehyde (13.0 mL, 128 mmol, 1.50 equiv) was then added in one portion, followed by formic acid (98%, 6.4 mL). The reaction was allowed to stir 48 h at 23 °C, during which time the product precipitated as a white solid. which was isolated via Büchner funnel filtration and purified via trituration with water and diethyl ether. After drying in vacuo, 7a was obtained as a white solid (23.6 g, 80%).二 A 250-mL, 3-neck flask was charged with anhydrous potassium carbonate (12.4 g, 90.0 mmol, 6.00 equiv) and anhydrous sodium sulfate (15 g). The solids were placed under vacuum and flame-dried. Once cool, 7a (5.2 g, 15 mmol, 1.0 equiv) was added under a positive stream of nitrogen, followed by anhydrous tetrahydrofuran (140 mL). The flask was capped with a water-cooled reflux condenser under an atmosphere of nitrogen and heated to reflux with stirring. After 15 h, the reaction was cooled to ambient temperature and the solids removed via filtration through a fine, glass frit. The filtrate was concentrated in vacuo and dried under high vacuum to give imine as a colorless oil |
6楼2010-11-08 20:24:51
寒月龙飞
木虫 (小有名气)
- 应助: 0 (幼儿园)
- 金币: 1789.1
- 帖子: 214
- 在线: 105小时
- 虫号: 346841
- 注册: 2007-04-15
- 性别: GG
- 专业: 化学生物学与生物有机化学
7楼2010-11-08 20:26:23