Water → (2,4-Dichloroanilino)acetonitrile

Chloroacetonitrile (40 ml) and 2,4-dichloroaniline (81.0 g) were heated with stirring in a 250 ml round-bottomed three-necked flask at 120°-125° C. for 1.0 hour and then for approximately 1 hour at 140°-145° C. The reaction mixture was cooled, diluted with CH2Cl2, and then placed in a separatory funnel and water added. Shaking the mixture resulted in crystal formation. The mixture was filtered and 39.2 g of 2,4-dichloroaniline hydrochloride removed. The CH2Cl2 layer was then separated from the filtrate and the CH2Cl2 layer treated with diatomaceous earth and activated charcoal and then filtered. The CH2Cl2 was then evaporated off, leaving a black viscous gum which on cooling with stirring solidified. Recrystallization from carbon tetrachloride gave 21.5 g of 2,4-dichloroanilinoacetonitrile.

1. waitfor approximately 1 hour at 140°-145° C
2. temperatureThe reaction mixture was cooled
3. customplaced in a separatory funnel
4. stirringShaking the mixture
5. customresulted in crystal formation
6. filtrationThe mixture was filtered
7. custom39.2 g of 2,4-dichloroaniline hydrochloride removed
8. customThe CH2Cl2 layer was then separated from the filtrate
9. additionthe CH2Cl2 layer treated with diatomaceous earth and activated charcoal
10. filtrationfiltered
11. customThe CH2Cl2 was then evaporated off
12. customleaving a black viscous gum which
13. temperatureon cooling
14. stirringwith stirring solidified
15. customRecrystallization from carbon tetrachloride

ORDレコード

ord-99a0000fae0f48d98f7fb3635f669980

出典データセット

uspto-grants-1982_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04343810