1-Methylpiperazine → HCID 21449882, compound

HRID 596442Notes

Reaction equation

HRID 596442 reaction equation
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:4]=2[CH2:3]1.[CH3:19][N:20]1[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]1>C(Cl)(Cl)Cl>[F:13][C:10]1[CH:11]=[CH:12][C:7]2[S:6][C:5]3[CH:14]=[C:15]([CH3:18])[CH:16]=[CH:17][C:4]=3[CH2:3][CH:2]([N:23]3[CH2:24][CH2:25][N:20]([CH3:19])[CH2:21][CH2:22]3)[C:8]=2[CH:9]=1

Participants

4

Reactant 2

HCID 531671-MethylpiperazineHCID 21416157HCID 21416157, compound

Product 1

HCID 21449882HCID 21449882, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

10.6 g. of 10-chloro-8-fluoro-10,11-dihydro-3-methyldibenzo[b,f]thiepin, 200 ml. of chloroform and 11.4 g. of N-methylpiperazine are heated at reflux for 30 hours. The mixture is evaporated under reduced pressure. The resulting residue is worked up via the neutral portion in essentially the same manner as described in Example 1, and there is obtained 1-{8-fluoro10,11-dihydro-3-methyl-dibenzo[b,f]thiepin-10-yl}-4-methylpiperazine, having a melting point of 117°-121° C. By treatment with methanesulfonic acid, there is obtained the dimethanesulfonate having a melting point of 176°-178° C. (from methanol/ether.

Workup

  1. temperatureat reflux for 30 hours
  2. customThe mixture is evaporated under reduced pressure

Sources & evidence

ORD record
ord-1502a58978064ed6b91af6ce12554753
Source dataset
uspto-grants-1977_03
Patent number
US04011222

Reaction notes

Loading…