Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexylamine | HCID 7965 | — |
| Reactant | HCID 10255676 | HCID 10255676 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10403249 | HCID 10403249 | 177.3% |
Reaction Steps
A solution of nitro acid of Example 8 (928 g; 4.35 mol) in ethyl acetate (9.6 L) was dried by atmospheric azeotropic distillation at constant volume. After cooling the solution to 40° C., cyclohexylamine (423 g; 4.26 mol) was added over 15 minutes. The resultant slurry was cooled to 20° C. over 4 hours and left to stir for 13 hours at 20° C. The solid was collected by filtration and the damp filter cake washed with ethyl acetate (1.3 L). The isolated solid was then dried in vacuo at 30° C. for 18 hours to give the title compound as a white solid (1.205 Kg) in 91% yield.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07018818B2 |
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| Source dataset | uspto-grants-2006_03 |
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| ORD ID | ord-dc9e379f47a846cab451df7e49f63a6a |
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| Source note | uspto-grants-2006_03 |
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