1-Methylpiperazine → HCID 21449882, compound

HRID 1658745Notes

Reaction equation

HRID 1658745 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-fluoro-10,11-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-c9d8adbbd8194fadabb6e90cc13b2db3
Source dataset
uspto-grants-1976_06
Patent number
US03966737

Reaction notes

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