X-Ray diffraction is an important and powerful tool for determining the solid state structure of compounds. Modern advances have made data collection and structure solution almost routine for many small molecules To use this technique, however, good quality single crystals are still needed. In this exercise you will experiment with the art of growing single crystals

For a two-solvent recrystallization, you should have one solvent (solvent #1) in which your desired compound is soluble at the boiling point. The second solvent(solvent #)should induce crystallization when added to a saturated solution of your compound in the primary solvent. Reference:

Working on a vacuum manifold: See LLP chapter 9.2 for an excellent discussion on working with air-sensitive reagents, including how to use a two-way manifold. De-gassing solvents: The best way to remove water and oxygen from a solvent is to distill it over an appropriate drying agent (such as sodium). This can sometimes be a lengthy (and dangerous)task. Since we

Overview: A good 'H NMR sample contains about 10 mg of compound. The solution should contain no solids or paramagnetic impurities. Your deuterated NMR solvent should be free of water,and your NMR spectrum should contain no solvent peaks. Reference: Zubrick page 295 is relatively useful, but you should follow the specifics in this handout Also, keep in mind that we won't be running continuous wave spectrometers, so you should disregard any discussion of them. NMR Solvents:

Flash column chromatography is a quick and (usually) easy way to separate complex mixtures of compounds. We will be performing relatively large scale separations in 5.301,around 1.0 g of compound. Columns are often smaller in scale than this and some of you will experience these once you move into the research lab. Column chromatography uses the same principles

WARNING NOTICE: The erperimants described in these matcrials are potantially hazardous and require a high level ofsafcty training special facilities and equipment, and supervision by appro responsibility, liability, and risk for the implemontation of such safey procedures and meastncs. MIT shall have no responsibility, liability, or risk for the content or implementation any of the matainl presented. Legal Notices

要熟悉流管柱层析法需要适当的练习。此影片将会让从你填充 的适当条件技巧开始、填充及进行管柱层析,甚至用管子做一个微 管柱层析。 It takes considerable practice to master the art of \running a column\. This video will get you started, with tips on picking appropriate conditions, packing and running a column, monitoring separation, and even making a micro-column from a pipet

在本影片中学习如何熟悉滴定技术---用酚?在酸/碱滴定中的详 细示范。 Learn how to master the art of titration in this video-with a detailed demonstration of an acid/base titration using phenolphthalein

薄层分析法在许多研究实业室是最常用的此影片将带领你每 步骤,从准备跑瓶到计算RF(retention factor)值 步骤, Thin-layer chromatography is the most commonly used analytical technique in many research labs. This video walks you through every step from setting up a developing chamber to calculating Rf values

萃取、冲洗和干燥:还没到结束不能算结束。藉由分液漏斗示 。 范液相-液相萃取并学习如何用”反应检查步骤”检查你的反应。这 是一个你不会想错失的一个纯化技巧! Extracting, Washing and Drying: It ain't over 'til it's over. Learn how to \work up\ your reaction using a separatory funnel to perform a liquid-liquid extraction. This is one purification technique you don't want to miss!