Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 1-Butanol | HCID 263 | — |
| Reactant | Ethyl 2-cyano-2-(1-cyanocyclopentyl)acetate | HCID 16226777 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | Phenylcyanoguanidine | HCID 53954996 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178510038 | HCID 178510038 | — |
Reaction Steps
2000 ml of n-butanol and 192.8 g of potassium-tert-butoxide were added to the reaction vessel at 45±5° C. and stirred for 30 mins. To the reaction mixture was added 194.42 g of ethylcyano acetate over 15 min and added 250 ml of n-butanol. The reaction mixture was heated to 60±5° C. under stirring and 250 g of N-cyanophenyl guanidine was added, followed by 250 ml of n-butanol and further heated to 93±3° C., maintained the same at 4 hrs with stirring. After completion of the reaction, the reaction mixture was cooled to 75±5° C. and 1750 ml of water was added and stirred at the same temperature for 30 mins. Further to the reaction mass was added 250 ml of glacial acetic acid; stirred and cooled to room temperature (RT). The resulting solid was filtered and washed with 500 ml of water, followed by washing with methanol and drying to yield the titled compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08653266B2 |
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| Source dataset | uspto-grants-2014_02 |
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| ORD ID | ord-81e4b4559dbc43efa57fb86a25cc0d0f |
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| Source note | uspto-grants-2014_02 |
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