Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethyl Bromide | HCID 6332 | — |
| Reactant | 3H-Pyrazol-3-one, 2,4-dihydro-5-methyl- | HCID 319771 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Product | ST001145 | HCID 668049 | — |
Reaction Steps
A mixture of 49 g 3-methyl-3-pyrazolin-5-one and 60.0 g bromoethane was sealed in a glass pressure tube and heated in an oil bath at 130° C. for 40 hours. After cooling, the tube was opened and the contents were poured into 200 g ice-water. Sodium bicarbonate (42.00 g) was added in small portions with stirring. The resulting mixture was stirred and heated to 100° C. for 1 hour, cooled to room temperature, and extracted with 10×50 ml portions of chloroform. The combined extracts were dried over anhydrous calcium chloride, evaporated under reduced pressure and the residue recrystallized from ethanol to give 20.1 g as colorless prim, m.p. 112°-113° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05461155 |
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| Source dataset | uspto-grants-1995_10 |
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| ORD ID | ord-027107efee7640ee8373a294ef281c6f |
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| Source note | uspto-grants-1995_10 |
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