1-Piperazinecarboxylic acid, ethyl ester → HCID 21456042, compound

HRID 435670Notes

Reaction equation

HRID 435670 reaction equation
Cl[CH:2]1[C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:13]=[CH:14][C:15]([CH3:17])=[CH:16][C:4]=2[CH2:3]1.[C:18]([N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1)([O:20][CH2:21][CH3:22])=[O:19]>C(Cl)(Cl)Cl>[C:18]([N:23]1[CH2:28][CH2:27][N:26]([CH:2]2[C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=3[S:6][C:5]3[CH:13]=[CH:14][C:15]([CH3:17])=[CH:16][C:4]=3[CH2:3]2)[CH2:25][CH2:24]1)([O:20][CH2:21][CH3:22])=[O:19]

Participants

4

Reactant 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 12539110HCID 12539110, compound

Product 1

HCID 21456042HCID 21456042, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

19.7 g of 10-chloro-10,11-dihydro-2-methyl-dibenzo-[b,f]thiepine dissolved in 100 ml of chloroform are heated under reflux for 24 hours together with 36.5 g of 1-carbethoxy-piperazine. Then the mixture is concentrated under reduced pressure and the residue crystallised from acetone/hexane. There is obtained 1-carbethoxy-4-(10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine of melting point 96°-98° C.

Workup

  1. temperatureare heated
  2. concentrationThen the mixture is concentrated under reduced pressure
  3. customthe residue crystallised from acetone/hexane

Sources & evidence

ORD record
ord-329d8f0fb5e746959c77460f0db4ad39
Source dataset
uspto-grants-1977_02
Patent number
US04006144

Reaction notes

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