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小熊小强金虫 (正式写手)
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[求助]
TTC合成
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Synthesis of S-1-Dodecyl-S′-( , ′-dimethyl- ′′-acetic acid)trithiocarbonate, 2. 1-Dodecanethiol (80.76 g, 0.40 mol), acetone (192.4 g, 3.31 mol), and Aliquot 336 (tricaprylylmethylammonium chloride, 6.49 g, 0.016 mol) were mixed in a jacketed reactor cooled to 10 °C under a nitrogen atmosphere. Sodium hydroxide solu- tion (50%) (33.54 g, 0.42 mol) was added over 20 min. The reaction was stirred for an additional 15 min before carbon disulfide (30.42 g, 0.40 mol) in acetone (40.36 g, 0.69 mol) was added over 20 min, during which time the color turned red. Ten minutes later, chloroform (71.25 g, 0.60 mol) was added in one portion, followed by dropwise addition of 50% sodium hydroxide solution (160 g, 2 mol) over 30 min The reaction was stirred overnight. 600 mL of water was added, followed by 100 mL of concentrated HCl (caution! gas, odor) to acidify the aqueous solution. Nitrogen was purged through the reactor with vigrous stirring to help evaporate off acetone. The solid was collected with a Buchner funnel and then stirred in1Lof 2-propanol. The undissolved solid was filtered off and was identified as S,S′-bis(1- dodecyl)trithiocarbonate. The 2-propanol solution was concentrated to dryness, and the resulting solid was recrystallized from hexanes to afford 92.5 g of yellow crystalline solid; mp 62 3 °C. IR (KBr): 1725, 1075. H NMR: 0.99 (t, 3H), 1.37 1.47 (m, 20H), 1.75 (s, 6H), 3.42 (t, 2H), 13.05 (s, 1H). MS (MH , chem. ion.): calcd for C17H33O2S3: 365.1642. Found: 365.1626. 快疯了，合成了九次，全军覆没！！！！！！！！！ |
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季燕军xiaoya
金虫 (小有名气)
- 应助: 16 (小学生)
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- 注册: 2012-10-08
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- 专业: 高分子合成化学
【答案】应助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
感谢参与，应助指数 +1
小熊小强: 金币+5, ★有帮助, 这个方案我试过，找到关键原因了，多谢参与！ 2013-04-19 08:44:35
小熊小强: 金币+15, ★有帮助 2013-04-19 16:42:27
感谢参与，应助指数 +1
小熊小强: 金币+5, ★有帮助, 这个方案我试过，找到关键原因了，多谢参与！ 2013-04-19 08:44:35
小熊小强: 金币+15, ★有帮助 2013-04-19 16:42:27
将计量好的十二硫醇(16.15g)、丙酮(38.5g)、相转移剂四丁基硫酸氢铵(2g)加入到500ml的三口烧瓶中，在氮气氛围下冷却至10℃。向烧瓶中滴加质量分数50％的氢氧化钠溶液6.7g，滴加10～15min。滴加完后，搅拌15min。10min内向三口烧瓶中滴加二硫化碳(6.1g)和丙酮(8.1g)的混合溶液，搅拌10min。溶液变为橙红色。向三口烧瓶中一次性加入氯仿14.25g后，30min内滴加质量分数50％的氢氧化钠32g，搅拌过夜。向三口烧瓶中加入120ml去离子水，随后加入20ml浓盐酸(注意产生的含硫气体的味道)，同氮气，剧烈搅拌，使反应物中的丙酮全部挥发。过滤后，固体产物用200ml异丙醇溶解，过滤除去不溶物。浓缩后，用正己烷结晶，得到s-1-十二烷基-s(α, α'-二甲基-α"-乙酸)三硫代碳酸酯(TTC),试试这个呢，我没做过 |
2楼2013-04-17 16:51:09