Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | HCID 86708474 | HCID 86708474 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89919757 | HCID 89919757 | 98.5% |
Reaction Steps
(I11C): To the stirred solution of 3-amino-4-chloro-5-(piperazin-1-yl)benzonitrile (1.0 g, 4.22 mmol) in dichloromethane (10 mL) was added BOC2O (0.981 mL, 4.22 mmol) at 0° C., drop wise over a period of 10 minutes followed by triethylamine (0.883 mL, 6.34 mmol). The reaction mixture was allowed to warm to room temperature, stirred it for 1 hour. The reaction mixture was diluted with methylene chloride (100 mL), washed with brine (30 mL), dried over Na2SO4 and concentrated at 45° C. to get tert-butyl 4-(3-amino-2-chloro-5-cyanophenyl)piperazine-1-carboxylate (1.4 g) as a brown solid. The crude material was washed with diethyl ether four times and dried under vacuum to get tert-butyl 4-(3-amino-2-chloro-5-cyanophenyl)piperazine-1-carboxylate (1.4 g) as an off-white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08940736B2 |
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| Source dataset | uspto-grants-2015_01 |
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| ORD ID | ord-498138a80e274f97a6560983c15e5bc5 |
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| Source note | uspto-grants-2015_01 |
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