Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 23332731 | HCID 23332731 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23332767 | HCID 23332767 | — |
Reaction Steps
Four grams (0.0123 mole) of the compound of Example 27, 3.81 ml (0.0369 mole) of diethylamine and 80 ml of dimethylformamide were heated at 80° C. for 6 hours. After evaporating the solvent, the reaction mass was taken up with chloroform, and the obtained organic solution was first washed with a saturated aqueous solution of sodium carbonate and then with water (twice). After drying over sodium sulfate, the chloroform was evaporated off and the obtained residue was passed through a silica-gel column by eluting with chloroform:methanol=99:1 (by volume). The obtained product was finally dissolved in diethyl ether and treated with a saturated solution of hydrogen chloride in diethyl ether whereby the title compound crystallized out. Yield 3.7 g. (76%). M.p. 252°-56° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04232017 |
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| Source dataset | uspto-grants-1980_11 |
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| ORD ID | ord-c5c99d168c7c44b3a44d86fd601bc8bf |
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| Source note | uspto-grants-1980_11 |
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