Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | 1-Heptyne | HCID 12350 | — |
| Reactant | Propionyl chloride | HCID 62324 | — |
| Reactant | Sodium | HCID 5360545 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 4663481 | HCID 4663481 | — |
Reaction Steps
A 1-liter reactor was loaded with 345 mL of diglyme (RN 111-96-6) and 17.2 g (748 mmoles) of sodium (RN 7440-23-5) cut into pieces. After heating to a temperature slightly above the melting point of sodium accompanied by thorough stirring, 71.7 g (745 mmoles) i.e. 97.5 mL of 1-heptyne (RN 628-71-7) in solution in 100 mL of diglyme is then added four times at hourly intervals. The medium thickens to form a beige suspension. Stirring is continued for another 2 hours 30 minutes at the same temperature. The mixture is cooled down to 25-30° C. and poured slowly into a stirred solution of 64.8 g (700 mmoles) i.e. 61.0 mL of propionyl chloride (RN 79-03-8) in 600 mL of ethyl ether. An exothermic reaction takes place followed by stirring for 1 hour at no particular temperature.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09265852B2 |
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| Source dataset | uspto-grants-2016_02 |
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| ORD ID | ord-38c0e2f352b648e7aac24b9446acdb60 |
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| Source note | uspto-grants-2016_02 |
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