Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 178490529 | HCID 178490529 | — |
| Solvent | Methyl Isobutyl Ketone | HCID 7909 | — |
| Product | HCID 178490547 | HCID 178490547 | — |
Reaction Steps
40 ml of a 50% aqueous dimethylamine solution was added to a solution of 2 g of N-(cis-4-methylcyclohexyl)-4-(2-chloroethoxy)-3-methoxycinnamamide (Example 106) in 40 ml of methylisobutylketone. The solution was reacted for 18 hours by heating heated to 110° C., in a closed system. After reaction, the reaction solution was added with 200 ml of an aqueous sodium chloride solution and 100 ml of methylene chloride, and subjected to extraction. The aqueous layer was extracted twice with 100 ml of methylene chloride. The organic layer obtained was washed twice with an aqueous sodium chloride solution and dried over magnesium sulfate. Thereafter, the solvent was removed in vacuo. The product obtained was recrystallized from methylene chloride/ether, yielding 1.6 g of N-(cis-4-methylcyclohexyl)-4-(2-dimethylaminoethoxy)-3-methoxycinnamamide (a compound of the present invention) as white crystal, which had the following physiochemical properties:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05344845 |
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| Source dataset | uspto-grants-1994_09 |
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| ORD ID | ord-0bab9d4f06334f5b8376b601ec58a1df |
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| Source note | uspto-grants-1994_09 |
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