Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 53719602 | HCID 53719602 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | Hydrogen Bromide | HCID 260 | — |
| Product | HCID 23450657 | HCID 23450657 | — |
Reaction Steps
Under a slight stream of nitrogen, 19.0 g of (2-chloro-allyl)-dithiocarbamic acid cyclohexyl ester are placed in 100 ml of acetonitrile and cooled to 0-1° C. Before and during the addition of bromine, the apparatus is flushed thoroughly with nitrogen. Then 14.0 g of bromine are added in the course of 70 minutes in such a manner that the temperature can be maintained at 0-10° C. When the addition is complete, stirring is carried out for about 20 minutes. The reaction mixture is concentrated in vacuo at 20-25° C. 50 ml of hexane are added to the crude product, and the product is filtered off with suction at 20-25° C., washed twice with 45 ml of hexane and dried in vacuo at room temperature. The title product is obtained in the form of the hydrobromide (compound 2.3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06677457B2 |
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| Source dataset | uspto-grants-2004_01 |
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| ORD ID | ord-6617998a3cbb493fb22ddb0f2e244415 |
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| Source note | uspto-grants-2004_01 |
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