HCID 20575145, compound → HCID 20575169, compound

HRID 894317Notes

Reaction equation

HRID 894317 reaction equation
Cl.[S:2]1[CH:6]=[CH:5][C:4]([C:7]([C:15]2[CH:19]=[CH:18][S:17][CH:16]=2)=[C:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)=[CH:3]1>CO>[S:2]1[CH:6]=[CH:5][C:4]([CH:7]([C:15]2[CH:19]=[CH:18][S:17][CH:16]=2)[CH:8]2[CH2:13][CH2:12][N:11]([CH3:14])[CH2:10][CH2:9]2)=[CH:3]1

Participants

3

Reactant 1

HCID 20575145HCID 20575145, compound

Product 1

HCID 20575169HCID 20575169, compoundYield 11%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

9.5 grams (0.03 mole) of 4-(di-3-thienyl-methylene)-N-methyl-piperidine hydrochloride were dissolved in 270 ml of methanol and hydrogenated in the presence of 9.5 grams of PdBaSO4 (9.25% Pd) at 65° C. and 5 bar. The purification was carried out by dry column chromatography on silica gel (elution agent: chloroform/methanol=95%/5% by volume) and recrystallization from chloroform/petroleum ether. M.P. of the hydrochloride 251°-253° C.; Yield: 11%.

Workup

  1. customThe purification
  2. customby dry column chromatography
  3. customon silica gel (elution agent: chloroform/methanol=95%/5% by volume) and recrystallization from chloroform/petroleum ether
  4. customM.P. of the hydrochloride 251°-253° C.

Sources & evidence

ORD record
ord-6f14c2546fa547a5b0c03797b95c91d7
Source dataset
uspto-grants-1981_08
Patent number
US04283405

Reaction notes

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