Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Sodium Cyanate | HCID 517096 | — |
| Reactant | 1-(Tetrahydro-2-furoyl)piperazine | HCID 2734641 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57066098 | HCID 57066098 | 82.3% |
Reaction Steps
4-(2-Tetrahydrofuroyl)piperazine (33.25 g, 180.7 mmol) (III) is dissolved in 165 mL water. 5N Hydrochloric acid (34.5 mL) is added and the suspension is heated to 70° C. with stirring. Sodium cyanate (13.1 g, 201.15 mmol) is added in small portion to the stirring solution and heating is continued for an additional 2 hours. The reaction mixture is concentrated under reduced pressure to yield a thick oil. Chloroform (100 mL) is added to the off and the solution is heated to reflux. The hot solution is filtered and the filtrate is dried over Na2SO4. The dried solution is concentrated under reduced pressure to a thick yellow oil. Ether (50 mL) is added to the oil and white crystals precipitated out. The product is filtered, washed with ether (25 mL) and dried. The product is used without further purification (33.8 g, 82.3% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05675006 |
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| Source dataset | uspto-grants-1997_10 |
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| ORD ID | ord-f0415c69f73f4eeeb6d03077f95deb14 |
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| Source note | uspto-grants-1997_10 |
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