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CAS No. : | 66247-84-5 | MDL No. : | MFCD13176517 |
Formula : | C4H8ClN3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 133.58 | Pubchem ID : | 45791344 |
Synonyms : |
|
TPSA :Topological Polar Surface Area | 54.7 | H-Bond Acceptor Count : | 2 |
XLogP3 : | - | H-Bond Donor Count : | 3 |
SP3 : | 0.25 | Rotatable Bond Count : | 1 |
Signal Word: | Warning | Class | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | N/A |
GHS Pictogram: |
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Yield | Reaction Conditions | Operation in experiment |
---|---|---|
100% | Stage #1: With ammonia In methanol at 40℃; for 0.50 h; Stage #2: With hydrogen In methanol at 40 - 50℃; for 28.00 h; Stage #3: With hydrogenchloride In methanol; diethyl ether |
12.0 g (124 mmol) 4-formyl-imidazole are placed together with 750 mg Raney nickel in 1000 ml of methanolic ammonia solution and shaken at 40° C. for 30 min. Then the mixture is hydrogenated in a Parr apparatus under a hydrogen atmosphere at 5 bars pressure at 40° C. for 14 h. Another 750 mg Raney nickel are then added and the mixture is again hydrogenated at 50° C. under a hydrogen atmosphere at 5 bars pressure for 14 h. The mixture is filtered, evaporated down i. vac., and in each case methanol, toluene and ethanol are added to the residue and it is again evaporated down completely i. vac. The residue is combined with ethereal hydrochloric acid in methanol and evaporated down completely i. vac. The residue is in each case combined with methanol and dichloromethane and evaporated down completely i. vac.Yield: 21.2 g (quant.)Rt value: 0.49 min (D)C4H7N3*2 HCl (170.04/97.12)Mass spectrum: (M+H)+=98 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
29% | With hydrogenchloride; hydrogen In tetrahydrofuran; ethanol; ethyl acetate at 80℃; for 3.00 h; | 18-1-3 C-(1 H-lmidazol-4-yl)methylamine dihydrochloride; To a solution containing 450 mg of piperidin-1 -yl-(1 -trityl-1 H-imidazol-4-yl- methylene)amine in 3.5 mL of 3N hydrogen chloride in ethyl acetate are added 90 mg of 10percent Pd/C, 0.5 mL of THF and 0.9 mL of ethanol. The reaction medium is placed under a hydrogen pressure of 6 bar and heated at 80°C for 3 hours. After filtering off the catalyst and evaporating off the solvents, the crude product obtained is chromatographed on silica gel (eluent: 6/4 DCIWMeOH). 50 mg of C-(1 H-imidazol- 4-yl)methylamine dihydrochloride in the form of a white powder are obtained in a yield of 29percent. |
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