WARNING NOTICE: The experiments described in these materials are potentially hazardous and require a high level ofsafety training, special facilities and equipment, and supervision by appropriate individuals. You bear the sole responsibility, liability, and risk for the implementation of such safety procedures and measures. MIT shall have no responsibility, liability, or risk for the content or implementation of any of the material presented. Legal Notices 1. Transfer and Extraction Techniques 1.1. Competent Chemist Rating:"Ethyl Ester's Excellent Adventure Techniques Checklist Extraction and Washing Careful transfer of solutions without loss of material Solvent drying and concentration Melting point determination Nuclear Magnetic Resonance(NMR)spectrometer operation Pre-lab Discussion and Required reading: Extraction: Zubrick Ch 15 LLP Ch. 10 Theory of extraction: Zubrick Ch 37 Melting point determination: Zubrick pp 87-92 NMR theory and operation: Zubrick Ch. 35, LLP Ch. 15.2 Digital Lab Techniques manual 5. Reaction Work-Up I: Extracting, Washing drying 6. Extraction Work-Up Il: USing the rotavap Equipment: Graduated Cylinder(100-mL) Separatory funnel(125-mL) Erlenmeyer flasks(2x250-mL) Beaker (150-mL) Round-bottomed flask(100-mL) NMR tube Funnel Filter Paper Rotary evaporator To manipulate and purify a known amount of a contaminated sample and to record its H NMR spectrum, all with minimal loss of material1. Transfer and Extraction Techniques 1.1. Competent Chemist Rating: “Ethyl Ester's Excellent Adventure” Techniques Checklist: • Extraction and Washing ❑ • Careful transfer of solutions without loss of material ❑ • Solvent drying and concentration ❑ • Melting point determination ❑ • Nuclear Magnetic Resonance (NMR) spectrometer operation ❑ Pre-lab Discussion and Required Reading: • Extraction : Zubrick Ch. 15, LLP Ch. 10 • Theory of extraction: Zubrick Ch. 37 • Melting point determination : Zubrick pp. 87-92 • NMR theory and operation : Zubrick Ch. 35, LLP Ch. 15.2 Digital Lab Techniques Manual: • 5. Reaction Work-Up I: Extracting, Washing & Drying • 6. Extraction Work-Up II: Using the Rotavap Equipment: • Graduated Cylinder (100-mL) • Separatory funnel (125-mL) • Erlenmeyer flasks (2x250-mL) • Beaker (150-mL) • Round-bottomed flask (100-mL) • NMR tube • Funnel • Filter Paper • Rotary evaporator Goal: To manipulate and purify a known amount of a contaminated sample and to record its 1 H NMR spectrum, all with minimal loss of material. 14 WARNING NOTICE: The experiments described in these materials are potentially hazardous and require a high level ofsafety training, special facilities and equipment, and supervision by appropriate individuals. You bear the sole responsibility, liability, and risk for the implementation of such safety procedures and measures. MIT shall have no responsibility, liability, or risk for the content or implementation of any of the material presented. Legal Notices