Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | HCID 25222139 | HCID 25222139 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 25222140 | HCID 25222140 | 98% |
Reaction Steps
To a suspension of 5.5 g of Fe in 30 mL EtOH was added slowly 2 mL 12 N HCl. The mixture was stirred at 75° C. for 1 hour. After cooling at 65° C., 12 mL 25% NH4Cl solution was added. The mixture was stirred 5 min and 6a (0.02 mol, in 5 mL EtOH) was added. The mixture is heated at 75° C. for 2 hour. After cooling to rt, 5 g celite was added the mixture was filtrated on celite and the remaining solids were washed several times with ethanol. The combined filtrates were concentrated and extracted with a CH2Cl2 and 10% Na2CO3. Concentration of the organic layer led to crystallisation of the amine IIb. Yield 98%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08450342B2 |
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| Source dataset | uspto-grants-2013_05 |
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| ORD ID | ord-c2bde66467d84d3aafaba31b86006278 |
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| Source note | uspto-grants-2013_05 |
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