Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pivaloyl chloride | HCID 62493 | — |
| Reactant | HCID 69245445 | HCID 69245445 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58585365 | HCID 58585365 | — |
Reaction Steps
0.66 ml of pivaloyl chloride are added dropwise to a suspension of 728 mg (1.18 mmol) of tert-butyl 4-[5-[(4′-hydroxy-1,1′-biphenyl-4-yl)oxy]-1-(4-methyl-phenyl)-6-oxo-1,6-dihydro-4-pyridazinyl]-1-piperazinecarboxylate (Example 46) and a catalytic amount of 4-DMAP in a mixture of dichloromethane (4.0 ml) and pyridine (0.4 ml) at room temperature. The heterogeneous reaction mixture is stirred at about 40° C. overnight. The slightly cloudy suspension is diluted with dichloromethane and washed with 0.2 N hydrochloric acid solution and saturated sodium chloride solution, dried over magnesium sulfate and concentrated. The crude product is purified by chromatography on silica gel.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07320977B2 |
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| Source dataset | uspto-grants-2008_01 |
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| ORD ID | ord-deb35b31a1b241de870eb79be7a39602 |
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| Source note | uspto-grants-2008_01 |
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