1-Piperazinecarboxylic acid, ethyl ester → HCID 21416131, compound

HRID 1075883Notes

Reaction equation

HRID 1075883 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][CH:10](Cl)[C:9]3[CH:13]=[C:14]([F:17])[CH:15]=[CH:16][C:8]=3[S:7][C:6]=2[CH:18]=1.[C:19]([N:24]1[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]>C(Cl)(Cl)Cl>[C:19]([N:24]1[CH2:29][CH2:28][N:27]([CH:10]2[C:9]3[CH:13]=[C:14]([F:17])[CH:15]=[CH:16][C:8]=3[S:7][C:6]3[CH:18]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=3[CH2:11]2)[CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]

Participants

4

Reactant 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 21416144HCID 21416144, compound

Product 1

HCID 21416131HCID 21416131, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

38.8 G. of 3,10-dichloro-10,11-dihydro-8-fluoro-dibenzo[b,f]thiepin into 100 ml. of chlorofrom are heated with 82 g. of 1-carbethoxypiperazine for 24 hours under reflux conditions. The reaction mixture is poured on ice water and equilibrated with chloroform. The organic phase is dried over magnesium sulfate and evaporated under reduced pressure, Raw 1-carbethoxy-4-(3-chloro-10,11-dihydro-8-fluoro-dibenzo[b,f]thiepin10-yl)-piperazine is obtained as a yellow oil.

Workup

  1. temperatureof chlorofrom are heated with 82 g
  2. dry with materialThe organic phase is dried over magnesium sulfate
  3. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-431863300ad04d039b9c0d55627eaf98
Source dataset
uspto-grants-1976_05
Patent number
US03954764

Reaction notes

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