The reaction involving chlorosulfonic acid and alkane (aryl) sulfonyl chloride

The reaction involving chlorosulfonic acid and alkane (aryl) sulfonyl chloride

Chlorosulfonic acid and sulfonyl chloride are often used in the preparation of organic intermediates through sulfonation reactions, and alk(aryl)sulfonyl chlorides are often introduced into intermediate compounds as strong leaving groups

1.

Chlorosulfonic acid and alkane (aryl) sulfonyl chloride have high density, are strong acids, have a strong corrosive effect on fabrics and human skin, and are also very toxic

2.

(1) Because chlorosulfonic acid and alkane (aryl) sulfonyl chloride have high density, strong corrosiveness and high toxicity, they should be put in a bucket for long-distance transfer, and two hands should be used for short-distance movement, one hand holds the bottle and one hand supports the bottom.

(2) There should be an exhaust gas absorption device, which should be absorbed by alkaline solution, and a buffer safety bottle should be built in the middle of the exhaust gas absorption device

(3) During post-processing, the cooled reaction liquid should be slowly poured into ice water under stirring to prevent exothermic flushing

Sodium (potassium) cyanide and its reactions

Sodium (potassium) cyanide is often used in the chemical laboratory for condensation, addition and introduction of cyano groups

1.

Sodium cyanide and potassium cyanide are both highly toxic drugs, and the former is much more toxic than the latter

(1) Skin contact: Take off contaminated clothing immediately, rinse thoroughly with running water or 5% sodium thiosulfate solution for at least 20 minutes, and then decide whether to send to a doctor according to the situation

(2) Eye contact: immediately lift the eyelids, rinse thoroughly with a large amount of running water or saline for at least 15 minutes, and then decide whether to send to a doctor according to the situation

(3) Inhalation: quickly leave the scene to a place with fresh air

(4) Ingestion: Drink enough warm water to induce vomiting

The CN ^- + of Na ₂ S ₂ O _.

2.

(1) Perform various operations in accordance with the "five-double system" of the national drug control policy
.

(2) Wear gas masks and gloves for personal protection when feeding, reacting and post-processing
.
Especially in the reaction under acidic conditions, HCN gas will overflow.
In addition to engineering protection, strict personal protection is also necessary
.
In the case of a large reaction volume, a portable hydrogen cyanide gas analyzer can be hung or worn at the operating station , and a more accurate "benzidine" small paper strip can be used for real-time monitoring
.

(3) For the Bucherer-Bergs reaction involving KCN and ammonium carbonate , it should be noted that ammonium carbonate is easy to sublime when heated, and condenses at the inner neck of the lower part of the condenser, which will cause blockage and cause rigid sealing, which will lead to an explosion
.
It is necessary to keep the condenser unobstructed, and people should not leave the post during the reaction, and the heating reaction should not be done overnight (unless someone is on duty)
.

(4) All utensils and post-treatment aqueous solutions that have been in contact with cyanide should be rinsed with NaClO in a fume hood
.
The pH of the waste liquid was adjusted to 11 with alkali, and the excess CN was quenched with NaClO.
About 500 mL of saturated NaClO solution was needed for excess 1 mol of cyanide
.
After stirring thoroughly, let it stand overnight .
The next day, use a cyanide test paper to measure the cyanide concentration, and it is safer if it is less than 10
.

Three, examples

Application process: Add 60g (0.
3mol) of the substrate, 29.
5g (0.
45mol) of potassium cyanide and 57g (0.
6mol) of ammonium carbonate to 1000mL of aqueous ethanol , and heat to 60℃ to react overnight.
.
.

Remarks: ①Be careful that the sublimation of ammonium bicarbonate can easily block the lower part of the condenser.
It is best to use a straight condenser and unblock it frequently: ②Wear gas masks and gloves for personal protection when feeding, reacting and post-processing; ③This The reaction heated to 60°C should not be left unattended and allowed to react overnight; ④All utensils and post-treatment aqueous solutions that have been in contact with cyanide should be rinsed with NaClO in a fume hood
.
Disposal of waste liquid should follow item (4) in the above safety operation precautions
.

Related links: Hydrogen sulfide and the reactions it participates in