Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-Bromobutyronitrile | HCID 21412 | — |
| Reactant | HCID 178507494 | HCID 178507494 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178511041 | HCID 178511041 | — |
Reaction Steps
A 2 mL CH3CN suspension of 0.05 g (0.11 mmol) 8-(2-aminobenzyl)-4-(cyclohexylamino)-1-(3-fluorophenyl)-1,3,8-triazaspiro[4.5]dec-3-en-2-one (example 80), excess 4-bromobutyronitrile and Cs2CO3 was heated to 60° C. and allowed to stir for 2 days. HPLC/MS showed a small amount of product so the reaction was filtered and concentrated. The remaining oil was purified on an Isco automated system affixed with a Biotage Flash 25(M) cartridge eluted with 0-5% MeOH+0.5M NH3 in CH2Cl2 over 30 min at 20 mL/min. The product eluted last.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08114887B2 |
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| Source dataset | uspto-grants-2012_02 |
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| ORD ID | ord-74aedacff2444845a379ad0cec80793f |
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| Source note | uspto-grants-2012_02 |
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