반응 #2006478

반응 방정식

Toluene

NaOH

5-amino-2-cyanobenzotrifluoride

phosgene

toluene

→

compound 8a

4-Isocyanato-2-trifluoromethyl-benzonitrile

용매

ethyl acetate

ethyl acetate

반응 조건

후처리

1. 1
   기타to return at room temperature
2. 2
   온도the resulting solution was refluxed for 3 hrs
3. 3
   기타The first 6 mL of distilled solvent was removed
4. 4
   여과The solution was then filtrated
5. 5
   기타evaporated

실험 절차

To a solution of 5-amino-2-cyanobenzotrifluoride (1a) (2.0 g, 10.7 mmol) in ethyl acetate (6 mL) at 0° C. under argon, was added dropwise a 2.0 M solution of phosgene in toluene (6.5 mL, 12.9 mmol). The solution was stirred 30 min at 0° C. and allowed to return at room temperature. Toluene (3 mL) was then added to the ethyl acetate and the resulting solution was refluxed for 3 hrs using a Dean-Stark apparatus, equipped with an HCl trap (solid NaOH). The first 6 mL of distilled solvent was removed and replaced by toluene (6 mL). The solution was then filtrated and evaporated to give compound 8a (1.6 g) as an orange oil which was directly used for the next step. IR: 2268 (strong), 2232 (weak) cm−1.

출처