Diethyl ether

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Legality: DEA Listed Chemicals

Production of this substance may be illegal in some jurisdictions under certain circumstances.

21CFR1310.02 a & b

In 1995/6, two lists were created "List I" and "List II", for which commercial manufacturers and distributors must register, and for which possession with the intent to manufacture illegal substances (such as methamphetamine, ecstasy, etc) is illegal. On these a few dozen "precursor" compounds commonly used in the manufacture of illegal drugs. [1] [2]

Bottom line: Do not produce this chemical without checking to make sure that you may do so legally.

 
 
Diethyl ether
DEA LIST I/II SUBSTANCE
Chemical formula (C2H5)2O
OTP appearance clear liquid 
Molar Mass(g/mol) 74.02 
Density(g/cc) 0.7134 
Melting Point(°C) -116.3 
Boiling Point(°C) 34.6
NFPA 704
NFPA704.png
4
2
1
 

Uses

Primary

  • As a solvent
  • As a liquid-liquid separator (see vinegar)
  • Pharmacopia: As an anesthetic

Other

Natural occurrence

Hazards

  • Diethyl ether is highly flammable and it forms peroxides which are explosive. Keep away from open flames.
  • Diethyl ether has a very low vapor pressure. It evaporates very easily. Keep it in sealed containers.
  • Diethyl ether depresses the central nervous system if inhaled. Do not inhale.
  • Diethyl ether is toxic in large quantities. Do not drink.
  • Diethyl ether is often stored over sodium metal. If a water-contaminated amount was returned to the storage vessel, it could explode.

This is all quite real. Be very very careful.

Production

Synthesis

  1. In a sand bath alembic, heat a mass of dry sulfuric acid to 100°C. Do not allow the temperature of the sulfuric acid to exceed 140°C.
  2. Add ethanol, drop by drop, to the sulfuric acid until all the ethanol is gone.

Side Reactions

Ethylene and acetaldehyde may also be produced by the sulfuric-acid-ethanol reaction.

  • Ethylene is favored when the reaction temperature gets too hot (> 140°C)
  • Acetaldehyde is favored when there is excess oxygen.

Both of these can be differentiated from diethyl ether by their odor.

Purification

One online source[3] gives this method:

  1. Combine 100ubm of diethyl ether with 12ubm of potassium hydroxide
  2. Stir overnight in warm conditions.
  3. Allow to settle/separate
  4. Decant ether layer
  5. Discard remainder
  6. Add 4ubm sodium metal shavings
    Na + H2O NaOH + H2 // dangerous!
  7. stir overnight or until sodium amalgamates completely
  8. distill ether

Testing

Storage

Store in air/water tight container over sodium metal to keep dry, or sodium hydroxide to prevent peroxide formation. Store below 30°C to prevent boiling and peroxide formation.

Disposal

  • Can be burned, if you're careful.

See Also

Working in a stirred vessel, potassium ethoxide in diethylaniline is used to catalyse addition of ethyl alcohol with acetylene. The reaction proceeds at 160-165°, and a column head temperature of 37 to 44° is maintained by adjusting the alcohol feed rate. Vinyl ethyl ether of 60% strength or higher is obtained according to the control exercised, and may be purified by fractional distillation, Washing with water, and drying. [4]

References

  1. "Emphasizing the "Control" in controlled substances"
    United States Drug Enforcement Agency
    link last accessed 11 September 2012.
  2. "Controlled Substances Act; Title 21; Chapter 13; Subchapter I"
    United States Food & Drug Administration
    link last accessed 11 September 2012.
  3. Purifying and Drying Diethyl Ether For Grignard Reactions Using Potassium Hydroxide and Sodium, by NurdRage
    courtesy YouTube.
  4. US patent 2404700 "MANUFACTURE OF VINYLETHERs"
    Link courtesy Google