C1C=CC=CC=1.[C:7]([C:11]1[CH:12]=[C:13]([OH:18])[CH:14]=[CH:15][C:16]=1[Cl:17])([CH3:10])([CH3:9])[CH3:8].[Cl:19][C:20](OC(Cl)(Cl)Cl)=[O:21].C(N(CC)CC)C>CCCCCC>[Cl:19][C:20]([O:18][C:13]1[CH:14]=[CH:15][C:16]([Cl:17])=[C:11]([C:7]([CH3:10])([CH3:8])[CH3:9])[CH:12]=1)=[O:21]Into 50 ml of benzene were dissolved 9.2 g of 3-tert-butyl-4-chlorophenol and 5.5 g of trichloromethyl chloroformate, and a solution obtained by dissolving 5.8 g of triethylamine into 20 ml of benzene was added dropwise thereto with stirring and cooling by ice. After completion of this dropwise addition, the mixture was subjected to stirring for 12 hours at room temperature. To the reaction mixture were added 70 ml of hexane, and precipitated crystal was separated by filtration. The filtrate was washed with water and a saturated aqueous solution of sodium chloride in this order, and was dried over anhydrous calcium chloride. Thereafter, solvent was distilled off. The residue was distilled under reduced pressure to give 9.32 g of 3-tert-butyl-4-chlorophenyl chloroformate having boiling point of 105°-108° C./1 mmHg, of which properties are as follows.
Wird geladen…
