Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 57827368 | HCID 57827368 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 67279256 | HCID 67279256 | — |
Reaction Steps
Thiourea (2.09 g) was added to a solution of 1-(2-chloromethylcyclohex-1-enyl)-2-fluorobenzene obtained in Preparation Example 1-(4) (5.88 g) in ethanol (200 mL). The reaction solution was heated to 80° C. and stirred for 270 minutes. Thiourea (399 mg) was added to the reaction solution, followed by stirring at the same temperature for one hour. After cooling to room temperature, the solvent was evaporated under reduced pressure. Diethyl ether and ethyl acetate were added to the residual syrup. A white solid was precipitated by ultrasonic treatment. After standing at room temperature for 30 minutes, the supernatant was removed. Further, the solid was washed with diethyl ether and the supernatant was removed again. The resulting solid was dried under reduced pressure to obtain the title compound (6.38 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08158620B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-88f24f019a0447148485de1440308abb |
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| Source note | uspto-grants-2012_04 |
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