1 -methyl-4-piperidyl

Amixture of 3.4 gof 10-methoxy-4-(1 -methyl-4-piperidyl)-4H-ben2o[4,5]cyclohepta[1,2-b]-thiophen-4-ol base and 40 cc of 3 N hydrochloric acid is kept in a boiling water bath at 95°C to 100°C for 1 hour. The mixture is subsequently made alkaline with concentrated caustic soda solution at 20°C while cooling, and the free base Is extracted with chloroform. The chloroform solution is concentrated, and the residue is recrystalli2ed from ethanol/water 1 1. The pure 4-(1 -methyl-4-piperldylidene)-4H-ben2o[4,5]cyclohepta[1,2-b] thiophen-10(9H)-one base, having a melting point of 152°C to 153°C, is obtained in this manner. 

Pentapiperfde. a-(l-Methylpropyt)benzeneacetic acid 1 -methyl-4-piperidinyl ester 3-methyl 2-phenylraleric acid l-methyl-4-piperidyl ester 2-phenyl -3-methylpentanoic acid 1-methyl-4-piperidyl ester 1 -methyl -4 -pipertdyl 3-methyl-2-phenylvalerate. C Hj-NO, mol wt 289.40. C 74.70%, H 9.40%, N 4.84%, O 11.06%. Prepn Brit. pat. 781,382 and Martin, Habicht, U.S. pat. 2,987,517 (1957, 1961 to Cilag). 

The chloroform solution is concentrated and the residue recrystallized from 270 cc of absolute ethanol. The pure 10-methoxy-4-(1-methyl-4-piperidyl)-4H-benzo[4,5] cyclohepta[1,2-b) -thiophen-4-ol base, having a melting point of 194°C to 196°C, is obtained in this manner. Microanalysis corresponds with the formula C20H23NO2S. 

Aj Preparation of 1 -Methyl-4-Piperidyl-Magnesium Chloride Magnesium turnings (5.45 g,... 

Bis(1-methyl-4-piperidyl)propane Bis(methylthio)methane 1,2-Bis(/ Amorpholino)ethane... 

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