Phosphorus pentachloride → HCID 21315986、化合物

反応式

[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3=[CH:12][S:13][CH:14]=[C:9]3[C:8](=O)[NH:7][C:6]=2[CH:16]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:18]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][C:10]3=[CH:12][S:13][CH:14]=[C:9]3[C:8]([Cl:18])=[N:7][C:6]=2[CH:16]=1

参加物

実験手順

A 4.62 g. portion of 7-methyl-thieno[3,4-b][1,5]benzoxazepin-10(9H)-one is reacted with 4.60 g. of phosphorus pentachloride in 88 ml. of toluene as described in Example 7, to give 7-methyl-10-chloro-thieno[3,4-b][1,5]benzoxazepine. To this is added 40 ml. of dry toluene, 4.8 g. of N-ethylpiperazine and 10 ml. of triethylamine. The reaction is heated at 100° C. overnight, concentrated to a thick oil and treated as described in Example 3 giving the base compound which is then converted to the hemifumarate, m.p. 208°-209° C.