WARNING NOTICE: The erperimants descnbed in these materials are potentially hao ardous and require a high level ofsafcty training special facilitics and equipment, and supervision by approprinte individuals. You bear the solc responsibility, liability, and risak for the implemcntation of such safdty procedunes and measures. MrT shall have no responsiblity, liability, risk for the content or implemcutation of amy of the matcrial presented. Legal Notices

This is two-day- experiment. Do not start this experiment unless you have two free lab days to complete it.*** Techniques Checklist: Picking the correct eluent Adsorbtion of a crude mixture onto silica gel Separating complex mixtures using gradient elution Pre-lab Discussion: Suggest limited list of eluent solvent systems Discuss sample adsorption and gradient elution strategies

described in these matorials arc potentinlly hazandous and require a high levd ofsafety training spccial facilitics and equip mant, and supervision by approp iate individuals. You bea the sole responsibility, lisbility, and risk for the implamnentation of such safcty procedures and mcasures. MIT shall have no respongibility, liability, or risk for the content or implementationc any of the material presanted. Legal Notices

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

dscnibed in these materials are potentially hazardous and require a high level ofsafcty training special facilitics and equ by approp lividuak You bear the sole responsibility, liability, and risk for the in plementation of such safety procedures and measures. MIT shall have no responsibility, liability, or risk for the content or implementation of amy of the matcrial presented. Legal Notices

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:

Thin Layer Chromatography (TlC) is an extremely useful technique for monitorin reactions. It is also used to determine the proper solvent system for performing separations using column chromatography. tLC uses a stationary phase, usually alumina or silica, that is highly polar(standard) or non-polar(reverse phase). The mobile phase is a solvent whose polarity you will choose. In 5.301, and in most lab

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: As you may discover, growing single crystals takes patience as well as an artful hand Crystallizations can be very sensitive to temperature and minor disturbances. Therefore, you will be encouraged to try several different temperatures using otherwise identical conditions, and to always find a quiet undisturbed location to promote crystal growth. Here are some tried and true tips to get

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!