Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Reactant | N-4-Boc-N-1-Cbz-2-piperazine carboxylic acid | HCID 2756777 | — |
| Reactant | Tetrahydrofuran heptane | HCID 21263495 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21098156 | HCID 21098156 | — |
Reaction Steps
To a cooled (−75° C.) solution of LDA 2M in heptane/THF (1.5 eq) in THF, a solution of 1-[(benzyloxy)carbonyl]-4-(tert-butoxycarbonyl)piperazine-2-carboxylic acid (Bigge et al, Tetrahedron Lett. 1989, 30: 5193) in THF was added dropwise at −75° C. After being stirred for 1 hour at −75° C., MeI (1.5 eq) was added. After 2 hours at −75° C. the reaction mixture was left warming to r.t., evaporated, diluted with AcOEt, washed with NaHCO3, water, brine and dried over Na2SO4. The crude was purified by flash chromatography on silica gel (petroleum ether/AcOEt, 85:15) to obtain the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07820660B2 |
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| Source dataset | uspto-grants-2010_10 |
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| ORD ID | ord-fda9dc696fa14e679f06d7a4584ae133 |
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| Source note | uspto-grants-2010_10 |
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