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CAS No. : | 655225-01-7 | MDL No. : | MFCD07367890 |
Formula : | C11H21BrN2O2 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | IWSFZKCIZFXAFT-UHFFFAOYSA-N |
M.W : | 293.20 | Pubchem ID : | 15946441 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302+H312+H332-H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
83.7% | With carbon tetrabromide; triphenylphosphine; In dichloromethane; at 20℃;Cooling with ice; | Carbon tetrabromide (1.681 g, 5.07 mmol) was dissolved in dichloromethane (17 ml), cooled with ice.thereTertiary butyl 4- (2-hydroxyMethyl) piperazine-1-carboxylate (1.062 g, 4.61 mmol), triphenylphosphine (1.329 g, 5.07 mmol), and stirred overnight at room temperature was added dichloromethane (11 ml). After the reaction, the solvent was evaporated. The residue was purified by silica gel column chromatography (SNAP ULTRA 25 g, hexane / ethyl acetate) to give the title compound (1.131 g, 83.7percent) as a yellow solid. |
78% | With carbon tetrabromide; triphenylphosphine; In dichloromethane; at 0 - 20℃; for 20h; | STEP A: A solution of tetrabromomethane (1.58 g, 4.7 mmol) in DCM (10 mL) is added dropwise (30 min) to the solution of N-Boc-piperazin-4-ethanol (1 g, 4.34 mmol) and triphenylphosphine (1.23 g, 4.7 mmol) in DCM (10 mL) at 0°C. The reaction is left at RT for 20 h. The organic solvent is removed under reduced pressure and the crude is purified by flash column chromatography (eluent petroleum ether/EtOAc) to give the expected compound (1 g, 3.38 mmol, Yield 78percent) as colourless oil. H1-NMR (CDCI3) delta (ppm): 3.41-3.47 (m, 6H); 2.81 (t, J=6.00 Hz, 2H); 2.48 (t, J=6.00 Hz, 4H); 1.46 (s, 9H) |
With carbon tetrabromide; triphenylphosphine; In tetrahydrofuran; | Example 63; l-{2-[4-(3,5-dimethoxybenzyl)piperazin-l-yl]ethyl}-3,3-bis(4-fluorophenyl)pyrrolidin-2- one; Example 63A; tert-butyl 4-(2-bromoethyl)piperazine-l-carboxylate; tert-Butyl 4-(2-hydroxyethyl)piperazine-l-carboxylate (5.76 g, 25.0 mmol) was dissolved in dry tetrahydrofuran (100 mL) and carbon tetrabromide (9.12 g, 27.5 mmol). A solution of triphenyl phosphine (6.62 g, 25.3 mmol) in dry tetrahydrofuran (25 mL) was added dropwise, and the mixture was stirred for 20 hours. The reaction was diluted with n- hexane (100 mL) and washed with a saturated NaHCO3 solution, water and brine, dried with MgSO4, filtered and concentrated. Silica gel chromatography eluting with ethyl acetate/hexanes 1 :4 gave the title compound. MS (DCI) m/z 295(M+H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
36% | With N-ethyl-N,N-diisopropylamine; at 30℃; for 72h;Inert atmosphere; | Example 24 tert-Butyl 4-(2-bromoethyl)piperazine-1-carboxylate A mixture of tert-butyl piperazine-1-carboxylate (5.0 g, 26.9 mmol), 1,2-dibromoethane (25 mL), DIPEA (3.5 g, 26.9 mmol) was stirred at 30° C. under argon for 72 h. The solvent was removed under reduced pressure and the residue was purified by column chromatography on silica gel (1-2percent methanol/dichloroethane) to afford the desired product (2.8 g, 36percent yield) as a solid. ESI-MS m/z: 293.1[M+1]+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | (1) 4-[2-(1-tert-Butyloxycarbonylpiperazin-4-yl)ethyl]-1-(4-methoxycarbonylmethylphenyl)piperazine Prepared from 1-(4-methoxycarbonylmethylphenyl)piperazine hydrochloride and <strong>[655225-01-7]2-(1-tert-butyloxycarbonylpiperazin-4-yl)ethyl bromide</strong>. Yield: 45percent of theory, Melting point: 161-180° C. (dec.) Mass spectrum: M+ =446 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With N-ethyl-N,N-diisopropylamine; In methanol; 1,2-dibromomethane; | EXAMPLE X 2-(1-tert-Butyloxycarbonylpiperazin-4-yl)ethyl bromide A solution of 1.0 g of 1-tert-butyloxycarbonylpiperazine and 0.7 g (0.005 mol) of N-ethyldiisopropylamine in 5 ml of 1,2-dibromomethane is allowed to stand at room temperature for 3 days and then concentrated to dryness in vacuo. The residue is purified by means of chromatography on a silica gel column, methylene chloride which initially contains 1percent and then 2percent of methanol being used as eluent. Yield: 0.6 g (38percent of theory), Mass spectrum: (M+H)+ =293/295 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Intermediate 22: 1 ,1-Dimethylethyl 4-{2-r6-amino-2-(butyloxy)-8-(methyloxy)-9H- purin-9-yl1ethyl)-1-piperazinecarboxylate; 2-(Butyloxy)-8-(methyloxy)-9H-purin-6-amine trifluoroacetate (131 mg, 0.373mmole) and potassium carbonate (185mg, 0.41 mmole) in DMF (1 ml) was stirred and heated at 60°C for 1 hour. A solution of 1 ,1-dimethylethyl 4-(2-bromoethyl)-1- piperazinecarboxylate (120mg, 0.41 mmole) in DMF (0.6ml) was added and the mixture stirred at 500C for 2.5 hours and then left at room temperature overnight. The mixture was heated at 500C for a further 4 hours and then quenched with water (10ml) and extracted with ethyl acetate (3x1 OmI). The combined organic extracts were dried over anhydrous sodium sulphate, filtered and evaporated. The residue was purified by silica gel chromatography eluting initially with chloroform:methanol 90:1 then 80:1 then 75:1 and finaly 60:1. Product-containing fractions were combined and evaporated to give the title compound as a yellow oily solid (168mg). 1H NMR (CDCI3): delta 5.66 (2H, d), 4.25 (2H, t), 4.05 (2H, t), 4.10 (3H, s), 3.35 (4H, broad s), 2.71 (2H, t), 2.46 (4H, broad s) 1.76 (2H, q) 1.48 (2H, q), 1.45 (9H, s) and 0.96 (3H, t). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With potassium tert-butylate; In tetrahydrofuran; at 75℃; for 18h; | Example 63B; tert-butyl 4-(2-(3,3-bis(4-fluorophenyl)-2-oxopyrrolidin-l-yl)ethyl)piperazine-l- carboxylate; To a solution of 3,3-bis(4-fluorophenyl)pyrrolidin-2-one (Example 58B, 1.37 g, 5.00 mmol) in tetrahydrofuran (30 mL) was added potassium t-butoxide (1.0 M in tetrahydrofuran) (7.5 mL, 7.5 mmol) followed by the product from Example 63A (1.47 g, 5.00 mmol). The reaction mixture was heated at 75 0C for 18 hours. The reaction was concentrated, diluted with ethyl acetate, washed with water and brine, dried with MgSO4, filtered and concentrated. The residue was purified with silica gel chromatography eluting with 3percent methanol/dichloromethane to give the title compound. MS (DCI) m/z 486.3(M+H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In ethanol;Reflux; | Step 1 : A mixture of lb (4.85g, 16.5mmol) and 9a (16.5g, 0.33mol) in ethanol (50mL) was heated under reflux overnight, then evaporated under high vacuum. The residue was re-dissolved in ethanol and the resulting precipitate was filtered off. The filtrate was concentrated and dried to give crude 9b (4.02g, ca. 100percent). |
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