反应 #2171040

ord-79e5e99ff7524cba8159a210af91f2c3

反应方程式

S=C(Cl)Cl
thiophosgene
c1c[nH]cn1
imidazole
CCCC1CCC(C2CCC(c3cc(F)c(N)c(F)c3)CC2)CC1
4-(4′-n-propylbicyclohexyl-4-yl)-2,6-difluorophenylamine
CCCC1CCC(C2CCC(c3cc(F)c(N=C=S)c(F)c3)CC2)CC1
4′-(3,5-difluoro-4-isothiocyanatophenyl)-4-n-propylbicyclohexyl

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.STIRRINGthe mixture is stirred at RT for 24 hours

实验过程

4.9 ml of thiophosgene are added dropwise over the course of 30 minutes at 15-25° C. to 18.4 g of imidazole in 150 ml of dichloromethane, and the mixture is stirred at RT for a further 2 hours. 15.8 g of 4-(4′-n-propylbicyclohexyl-4-yl)-2,6-difluorophenylamine (prepared as described in Examples 1a-1e) are subsequently added, and the mixture is stirred at RT for 24 hours. Conventional work-up gives 4′-(3,5-difluoro-4-isothiocyanatophenyl)-4-n-propylbicyclohexyl having the following properties: C 65 N 225.5 1; Δε 16.0; Δn 0.1990.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06716491B2uspto-grants-2004_04