Pre-Lab

Methylcyclohexene Pre Lab

Introduction:

The purpose of this lab is to create 4-Methylcyclohexene through microscale procedure, and determine the infrared spectrum of the product using salt plates.

Table of Chemicals:

Name | Structure | MW | Phys. Prop | Amount | Safety | Other |

4-methcyclohexanol | | 114.2 g/mol | | 1.5 ml | | |

Phosphoric acid | | | | .4 ml | | |

Sulfuric acid | | | | 6 drops | | |

Sodium sulfate | | | | Enough to dry | | |

Procedure:

Place 1.5 ml of 4-methcyclohexanol in a 5-ml conical vial and reweigh the vial. Add .4 ml of 85% phosphoric acid and 6 drops of sulfuric acid to the vial. Mix with a glass stirring rod, and add a spin vane. Assemble a distillation apparatus

Next, for the dehydration phase start circulating the cooling water in the condenser and heat the mixture until the product begins to distill (170 degrees). The distillation should take about 30-45 minutes. During the distillation, use a pipet to remove the distillate from the well of the Hickman Head. Transfer the distillate to a clean 3-ml vial. Continue the distillation until no more liquid is being distilled. You should be left with .5 ml of liquid. Wash with saturated sodium chloride.

For the isolation and drying phase, allow the layers to separate and remove the bottom layer. Using a dry pipet, dry the top layer with sodium sulfate. Place a stopper in the test tube and set it aside for 10-15 minutes to remove the last traces of water. Carefully transfer as much distillate as possible to a small tared vial with a cap. Lastly, determin the IR spectrum for your product.