1-Piperazinecarboxylic acid, ethyl ester → HCID 21416190, compound
Reaction equation
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]2[S:6][C:7]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=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:9]2[C:8]3[CH:12]=[C:13]([F:16])[CH:14]=[CH:15][C:7]=3[S:6][C:5]3[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][C:4]=3[CH2:10]2)[CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
24 G. of 2,10-dichloro-8-fluoro-10,11-dihydro-dibenzo[b,f]thiepin in 80 ml. of chloroform are heated together with 38.4 g. of 1-carbethoxy-piperazine under reflux conditions for 20 hours. The reaction mixture is poured over ice water and extracted with chloroform. The organic phase is dried over magnesium sulfate and evaporated under reduced pressure, whereby there is obtained oily 1-carbethoxy-4-(2-chloro-8-fluoro-10,11-dihydro-dibenzo [b,f]thiepin-10-yl)-piperazine.
Workup
- extractionextracted with chloroform
- dry with materialThe organic phase is dried over magnesium sulfate
- customevaporated under reduced pressure
Sources & evidence
- ORD record
- ord-65cd238713c445648f05f4ffcbccf6f4
- Source dataset
- uspto-grants-1976_05
- Patent number
- US03954764
Reaction notes
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