Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | tert-Butanol | HCID 6386 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | P,P-Diphenylphosphinic azide | HCID 199401 | — |
| Reactant | 6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazol-3-carboxylic acid | HCID 21929102 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86594005 | HCID 86594005 | — |
Reaction Steps
0.09 cm3 of triethylamine is added to a suspension of 0.25 g of 6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazol-3-carboxylic acid in 1.5 cm3 of toluene and 1.5 cm3 of tert-butanol. The solution obtained is heated to the reflux temperature and 0.12 cm3 of diphenylphosphonyl azide is added dropwise. Refluxing of the reaction mixture is continued for eight hours. After forty-eight hours at a temperature in the region of 20° C., the reaction mixture is concentrated to dryness under reduced pressure (13 kPa) and the residue is purified by flash chromatography on a column of silica [eluent: dichloromethane]. 0.06 g of tert-butyl [6,6-diphenyl-1-(4-toluenesulphonyl)-6,7-dihydro-1H-indazol-3-yl]carbamate is thus obtained in the form of a white foam, which is used directly, the characteristics of which are as follows:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07119115B2 |
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| Source dataset | uspto-grants-2006_10 |
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| ORD ID | ord-6f499a5d293149779e7c1f853f56485c |
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| Source note | uspto-grants-2006_10 |
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