Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 13674813 | HCID 13674813 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 13674838 | HCID 13674838 | 59.1% |
Reaction Steps
A mixture of 15 g (45 mmoles) of 1-[N-(2,6-dimethylphenyl)-methanesulfonamido]-2-methanesulfonyloxy-propane and 45 ml (31.9 g, 0.44 moles) of diethyl amine is heated at 150° C. for 5 hours in a steel bomb. The mixture is cooled, dissolved in 300 ml of diethyl ether, the solution is washed thrice with 50 ml of water, each, and then extracted thrice with 70 ml of ice-cold 1 n hydrochloric acid, each. The acidic solutions are combined, the traces of diethyl ether are removed under reduced pressure, and then the pH of the solution is adjusted to 9 with concentrated aqueous ammonia. The mixture is allowed to stand at +5° C. for one hour. The separated crystalline substance is filtered off, washed with water and dried. 8.3 g (59.1%) of 1-[N-(2,6-dimethylphenyl)-methanesulfonamido]-2-diethylamino-propane are obtained as a light beige, crystalline substance; m.p.: 58°-60° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04922021 |
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| Source dataset | uspto-grants-1990_05 |
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| ORD ID | ord-82c6db4d0d3e4489932a0fdbdd657328 |
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| Source note | uspto-grants-1990_05 |
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