1-Piperazinecarboxylic acid, ethyl ester → HCID 20328334, compound

HRID 1973098Notes

Reaction equation

HRID 1973098 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]=[CH:15][C:16]([CH3:18])=[CH:17][C:4]=2[CH2:3]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:2]2[C:8]3[CH:9]=[C:10]([F:13])[CH:11]=[CH:12][C:7]=3[S:6][C:5]3[CH:14]=[CH:15][C:16]([CH3:18])=[CH:17][C:4]=3[CH2:3]2)[CH2:26][CH2:25]1)([O:21][CH2:22][CH3:23])=[O:20]

Participants

4

Reactant 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 1227554310-Chloro-8-fluoro-10,11-dihydro-2-methyldibenzo[b,f]thiepin

Product 1

HCID 20328334HCID 20328334, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

24 G. of 10-chloro-8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin in 80 ml. of chloroform are heated under reflux for 20 hours with 38.4 g. of 1-carbethoxy-piperazine. The mixture is poured on to ice-water and extracted with chloroform. The organic phase is dried over magnesium sulfate, evaporated under reduced pressure, and there is obtained crude, oily 1-carbethoxy-4-[8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl]-piperazine.

Workup

  1. temperatureunder reflux for 20 hours with 38.4 g
  2. extractionextracted with chloroform
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-41517b8776cb4ead84da06a67951f849
Source dataset
uspto-grants-1976_12
Patent number
US03996229

Reaction notes

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