3,5-Dichlorophenyl isocyanate → 3,5-Dichloroaniline

Participants

Reaction Steps

The saccharide-bonded silica gel was dispersed into a mixture of 8 ml of anhydrous DMA-LiCl and 3 ml of pyridine, and 5 g of 3,5-dichlorophenyl isocyanate (this was formed from 3,5-dichloroaniline by an ordinary method) dissolved in 5 ml of DMA were added thereto and reacted at 80° C. in nitrogen for 12 hours. The presence of excess isocyanate groups in the reaction mixture was confirmed by the peak of C=N stretching vibration at 2,270 cm-1 in its IR spectrum. The saccharide-bonded, surface-treated silica gel was washed with tetrahydrofuran, methanol, acetone and hexane and dried in vacuum at 60° C. for 2 hours. The resultant compound was then subjected to IR spectrometry and elementary analysis. Results of elementary analysis are shown in Table 1.

Provenance & Evidence