آزمایش شماره 3

3and 5. di nitro benzoic acid derivative of the common alcohols, ethers and is phenyl polyurethane. Alpha-naphthyl polyurethane may also be used, but this test is used for more phenols

Preparation of 3 and 5 Diy nitro benzoate:

A combination of 3 and 5 January Nytrvbnzvyyl chloride with alcohol, the corresponding ester is obtained and the methods for primary alcohols, secondary and tertiary appropriate. Especially for Alklhayy that is dissolved in water and minor amounts of water may be useful.

• p. 368–375;

• https://en.wikipedia.org/wiki/3,5-Dinitrobenzoic_acid

Test method:

liquid alcohols:

2ml of alcohol in a dry test tube with about half a gram of 3 and 5 December nitro-benzoyl chloride mixture and gently boil it for 5 minutes. Add about 10 ml of distilled water and the solution is cooled in an ice bath until a solid product is obtained. The raw product collected and washed with 10 mL of 2% sodium carbonate and water solution - crystallized photos Atanvlmjdda.

) solid alcohols:

1g of solid alcohol in 5 ml of dry pyridine solution and half a gram of 3 and 5 December nitro benzoyl chloride to add it. Heat the mixture to reflux for 15 minutes Weights. The reaction mixture cooled and a cold solution of 5 ml of 5% sodium carbonate and 5 ml of water and pour. Keep cool in an ice bath to precipitate soluble form. By smooth Buchner funnel and wash. Then ethanol - water (recrystallization).

3and 5. di nitro benzoat

A)1 cc of alcohol in 3 ml of pyridine solution to dry and add to it half a gram of benzoyl chloride or Paranytrvbnzvyyl chloride. After the initial reaction, the mixture gently for 1 minute and then the flame temperature while stirring vigorously to pour in 10 cc of water. After settling of sediment, pour out the liquid above it. The remaining 5% were washed with 5 ml of sodium carbonate solution and separated by the filter paper and recrystallized with ethanol.

B) Naphthyl urethane derivatives of alpha (α - naphthyl urethane):E)

F) One gram of alcohol or phenol without water in a test tube and 5.0 ml of phenyl isocyanate to add it. If phenol compound is unknown, have reacted with 2 or 3 drops of pyridine or anhydrous ethanol amines catalyzed said. If the reaction was not done for its own solution on a steam bath for 5 minutes to warm up. The desired solution in a beaker containing ice, cold and human walls with your whisk scratch the glass, thereby accelerating the crystallization and crystallization. Polyurethane prepared by dissolving it in 5 ml of carbon tetrachloride, petroleum ether or recrystallization he

J) Derived Urethane: (2cc) 1gr alcohol + 5gr phenyl isocyanate mixture is put into a water bath, cooled and the resulting crystals after drying it gain its melting point.

K) Physical properties: crystalline deposits

O) Error factors: the presence of water in the reaction vessel that polyurethane is derived breaks down carbon dioxide gas is released

Derivative melting point is taken that we should be dry .nmy derivatives containing the solvent is not dry and take the exact melting point.

At all stages of testing should consider the amount of material quantities used in case of non-compliance leads to a lot of mistakes we do regent to be tested error. Phenyl isocyanate in the urethane derivative Baydalkl sector must be solved if it is not unknown for that matter can not be resolved melting point and melting point for phenyl isocyanate is

error

Derivative melting point is taken that we should be dry .nmy derivatives containing the solvent is not dry and take the exact melting point.

Phenyl isocyanate in the urethane derivative Baydalkl sector must be solved if it is not unknown for that matter can not be resolved melting point and melting point for phenyl isocyanate is.

Dinitrobenzoic acid

Phenylisocyanate

Phenylisocyanate is an organic compound typically abbreviated PhNCO. The molecule consists of a phenyl ring attached to the isocyanate functional group. It is a colourless liquid that reacts with water. Phenylisocyanate has a strong odor and tearing vapours, therefore it should be handled in the fumehood.

References

1. Jump up ^ Emmanuil I. Troyansky "Phenyl Isocyanate" in Encyclopedia of Reagents for Organic Synthesis, 2001 John Wiley & Sons doi:10.1002/047084289X.rp073

2. Jump up ^ Mukaiyama, Teruaki; Hoshino, Toshio (1960). "The Reactions of Primary Nitroparaffins with Isocyanates". Joual of the American Chemical Society 82: 5339. doi:10.1021/ja01505a017

MECANISM

Polyurethane

Safety

Phenyl isocyanate:
Identify risks:
Potential acute health effects:
In the case of inhalation is very dangerous. In case of skin contact (irritant), of eye contact (irritant), consumption is dangerous.
Slightly hazardous in case of skin contact. Exposure to overdo it, you Tvandmnjr to death. The potential effects of chronic: Non Asrsrtan: Not available. Mutagenic effects: mutagenic for bacteria and / or yeast.
First aid measures: Eye contact:
. For Czech and remove any contact lenses contact, eye immediately with plenty of water for at least 15 are.
Skin contact: . In case of contact, immediately wash skin with plenty of water.
Inhalation:
. If inhaled, remove to fresh air.
Storage: Storage:
Container in a cool, well ventilated hold.
Physical and chemical properties
. Physical state and appearance: Liquid
Odor: acrid
Molecular Weight: 119.13 g / mole
Color: Colorless to light yellow. Clear Clear
. Boiling point: 158 ° C (316.4 ° F) - 168 C.
Melting Point: -30 ° C (-22 ° F)

Chromatography...