Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | 3-Iodobenzylamine | HCID 97012 | — |
| Reactant | HCID 21923086 | HCID 21923086 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 21923026 | HCID 21923026 | — |
Reaction Steps
The operation is carried out as in Stage 2 of Example 3 starting from 200 mg of the product obtained in Stage 1 of Example 3 and 4 ml of butanol and using 0.123 ml of 3-iodo-benzenemethanamine in place of the benzylamine. Agitation is carried out at ambient temperature then the reaction medium is taken to a temperature of 80 to 85° C. for 22 hours, left to return to ambient temperature, diluted with 4 ml of isopropanol, left for three hours at a temperature of approximately 0° C., followed by separating, washing with 10 ml of isopropanol and drying at a temperature of approximately 50° C. After purification on silica eluting with cyclohexane/ethyl acetate/ methylene chloride in a proportion of 70/15/15, 235 mg of expected product is obtained in the form of white crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07208598B2 |
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| Source dataset | uspto-grants-2007_04 |
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| ORD ID | ord-d23d7c5603a14092863fb1e020c7e1f4 |
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| Source note | uspto-grants-2007_04 |
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