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

HRID 441998Notes

Reaction equation

HRID 441998 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 6212ChloroformSolvent2×

Procedure

38.8 G. of 3,10-dichloro-10,11-dihydro-8-fluoro-dibenzo[b,f]thiepin into 100 ml. of chloroform 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]thiepin-10-yl)-piperazine is obtained as a yellow oil.

Workup

  1. dry with materialThe organic phase is dried over magnesium sulfate
  2. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-d7376bec22984744b4bbb20a8b694651
Source dataset
uspto-grants-1977_08
Patent number
US04044010

Reaction notes

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