Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Bromobutyronitrile | HCID 21412 | — |
| Reactant | tert-Butyl 3-methylpiperazine-1-carboxylate | HCID 2756810 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 56785630 | HCID 56785630 | 75% |
Reaction Steps
To the stirred solution of tert-butyl 3-methylpiperazine-1-carboxylate (prepared according to procedure reported in US200876758A1, 2008, 5 g, 24.97 mmol) in N,N-dimethylformamide (50 ml) were added potassium carbonate (17.25 g, 125 mmol) and 4-bromobutanenitrile (2.98 ml, 30.0 mmol) at 25° C. The resulting solution was stirred at 25° C. for 16 h. The progress of the reaction was monitored by TLC. After completion of the reaction water (100 ml) was added and extracted with dichloromethane (3×60 ml). The combined extract was washed with brine (25 ml) and dried over sodium sulphate, filtered and concentrated to give crude compound. The crude compound was purified by column chromatography over silica gel (100-200) using 15% ethyl acetate in hexane to obtain the title compound (5 g, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09359367B2 |
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| Source dataset | uspto-grants-2016_06 |
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| ORD ID | ord-7b208adbed704a808b3aa8372bc88b98 |
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| Source note | uspto-grants-2016_06 |
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