Phosphorus pentachloride → HCID 21315969, compound
Reaction equation
[CH:1]1[S:2][CH:3]=[C:4]2[C:10]=1[C:9](=O)[NH:8][C:7]1[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=1[O:5]2.P(Cl)(Cl)(Cl)(Cl)[Cl:17]>C1(C)C=CC=CC=1>[Cl:17][C:9]1[C:10]2[C:4](=[CH:3][S:2][CH:1]=2)[O:5][C:6]2[CH:15]=[CH:14][CH:13]=[CH:12][C:7]=2[N:8]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A 1.08 g. portion of thieno[3,4-b][1,5]benzoxazepin-10(9H)-one and 1.15 g. of phosphorus pentachloride in 22 ml. of dry toluene are reacted as described in Example 1, giving 10-chloro-thieno[3,4-b][1,5]benzoxazepine. To this is added 10 ml. of toluene, 7.2 g. of N-ethylpiperazine and 25 ml. of triethylamine. The mixture is heated overnight at 100° C. and concentrated to dryness. The residue is treated as described in Example 3 providing the base compound as a foam which is converted to the fumarate, m.p. 215°-217° C.
Sources & evidence
- ORD record
- ord-52942123d39f482f8f0826488b3f8021
- Source dataset
- uspto-grants-1979_06
- Patent number
- US04157444
Reaction notes
Loading…