반응 #441997

반응 방정식

1,2-dichloroethane

6-amino-3-chloro-4-methoxybenzonitrile

1,2-dichloro-ethane

calcium carbonate

thiophosgene

→

3-Chloro-4-methoxy-6-isothiocyanatobenzonitrile

용매

water

반응 조건

후처리

1. 1
   workup.ADDITIONa mixture of 23 g
2. 2
   workup.ADDITIONAfter the addition the mixture
3. 3
   workup.STIRRINGis stirred for one hour at 0°-5° C.
4. 4
   workup.STIRRINGstirred for 6 hours at this temperature and finally at 35° C. for an hour
5. 5
   여과The reaction mixture is filtered
6. 6
   기타the organic layer separated
7. 7
   세척washed with dilute hydrochloric acid, water
8. 8
   건조dried (MgSO4)
9. 9
   기타The solvent is removed by evaporation
10. 10
    기타the residue used without purification in the next step

실험 절차

To a solution of 27.4 g. (0.15 mole) of 6-amino-3-chloro-4-methoxybenzonitrile in 150 ml. of 1,2-dichloro-ethane at 0°-5° C. is added with stirring a mixture of 23 g. (0.2 mole) thiophosgene, 100 ml. 1,2-dichloroethane, 20 g. (0.2 mole) calcium carbonate and 200 ml. of water. After the addition the mixture is stirred for one hour at 0°-5° C., warmed to 20° C. and stirred for 6 hours at this temperature and finally at 35° C. for an hour. The reaction mixture is filtered and the organic layer separated, washed with dilute hydrochloric acid, water and dried (MgSO4). The solvent is removed by evaporation and the residue used without purification in the next step.

출처