Réaction #58789

Équation de réaction

oxygen

aniline

NaI

2,2,2-trifluoroethanol

carbon monoxide

→

phenylisocyanate

Solvants

DCB

1,2-dichlorobenzene

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONare charged
2. 2
   Températurethe total pressure is maintained constant at 40 bars
3. 3
   TempératureThe reaction is maintained under constant
4. 4
   TempératureAfter 3 hours the reactor is cooled to room temperature
5. 5
   TempératureThe temperature is increased to 180° C. under atmospheric pressure
6. 6
   AutreThe vapors of TFE are separated
7. 7
   Autrecondensed

Mode opératoire

In a 1000 ml high-pressure stirred autoclave 15.5 g of aniline, 7.6 g of the [Co-tBu-Salen]/Silica catalyst of Example 2, 1.78 g of NaI and 488 g of 2,2,2-trifluoroethanol (TFE) are charged. The autoclave is pressurized with carbon monoxide and oxygen in a volumetric ratio of 19/1. The temperature is increased to 120° C. and the total pressure is maintained constant at 40 bars. The reaction is maintained under constant vigorous stirring for three hours. After 3 hours the reactor is cooled to room temperature, depressurized and 97.8 g of 1,2-dichlorobenzene (DCB) is charged in the reactor. The temperature is increased to 180° C. under atmospheric pressure. The vapors of TFE are separated, condensed, and reused in the following example. In the bottom of the reactor a mixture of DCB and phenylisocyanate is obtained. From this mixture pheylisocyanate is recovered by distillation with 99% w/w purity.

Source