Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Tris(hydroxymethyl)aminomethane | HCID 6503 | — |
| Reactant | Cycloheptyl isocyanate | HCID 3356886 | — |
| Reactant | HCID 24899506 | HCID 24899506 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 68866659 | HCID 68866659 | — |
Reaction Steps
Treat 1-(4-Chlorophenyl)-2-isopropyl-2,7-diazaspiro[3.5]nonane, Isomer A (0.015 g) in ClCH2CH2Cl (1 mL) and acetonitrile (1 mL) with cycloheptyl isocyanate (18 uL), and the resulting mixture stirred at RT for 424 h. P—S Trisamine (Argoonaut, 4.64 mmol/g) (120 g) and ClCH2CH2Cl (2 mL) were added and the resulting mixture was shaken to 20 h. The reaction mixture was filtered, the resin washed with CH2Cl2 (2 mL). The resulting filtrate was concentrated in vacuo and then placed on a silica gel plate (1000 u) and eluted with CH2Cl2:MeOH (95:5) to give of 1-(4-chlorophenyl)-2-isopropyl-2,7-diazaspiro[3.5]nonane-7-carboxamide, white residue (0.0208 g). Add MeOH (0.5 mL) and 0.1N HCl in MeOH (1 mL), and concentrate in vacuo to give the title compound, as a white solid (0.0222 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07638526B2 |
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| Source dataset | uspto-grants-2009_12 |
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| ORD ID | ord-1941e214b1f54504a708b8b3daac343c |
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| Source note | uspto-grants-2009_12 |
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