1-Piperazinecarboxylic acid, ethyl ester → 1-Carbethoxy-4-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

HRID 1075876Notes

Reaction equation

HRID 1075876 reaction equation
Cl[CH:2]1[C:8]2[CH:9]=[C:10]([S:13][CH3:14])[CH:11]=[CH:12][C:7]=2[S:6][C:5]2[CH:15]=[C:16]([O:19][CH3:20])[CH:17]=[CH:18][C:4]=2[CH2:3]1.[C:21]([N:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)([O:23][CH2:24][CH3:25])=[O:22]>C(Cl)(Cl)Cl>[C:21]([N:26]1[CH2:31][CH2:30][N:29]([CH:2]2[C:8]3[CH:9]=[C:10]([S:13][CH3:14])[CH:11]=[CH:12][C:7]=3[S:6][C:5]3[CH:15]=[C:16]([O:19][CH3:20])[CH:17]=[CH:18][C:4]=3[CH2:3]2)[CH2:28][CH2:27]1)([O:23][CH2:24][CH3:25])=[O:22]

Participants

4

Reactant 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 1282220110-Chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin

Product 1

HCID 134982441-Carbethoxy-4-(10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin-10-yl)-piperazine

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

24 G. of 10-chloro-10,11-dihydro-3-methoxy-8-methylthio-dibenzo[b,f]thiepin in 100 ml. of chloroform are heated with 55 ml. of 1-carbethoxypiperazine under reflux conditions for 20 hours. The mixture is poured on to ice/water and extracted with chloroform. The organic phase is dried over magnesium sulfate and evaporated under reduced pressure, whereby there is obtained crude 1-carbethoxy-4-(10,11-dihydro-3-methoxy-8-methylthiodibenzo[b,f]thiepin-10-yl)-piperazine.

Workup

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

Sources & evidence

ORD record
ord-6f38a79cdb88423f8ee2f036c9538325
Source dataset
uspto-grants-1976_05
Patent number
US03954764

Reaction notes

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