Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Methylcarbazole | HCID 20746 | — |
| Reactant | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| Catalyst | Benzyltributylammonium chloride | HCID 159952 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86629954 | HCID 86629954 | 96% |
Reaction Steps
To a solution of 3-methylcarbazole (500 mg, 2.76 mmol) in toluene (7.5 mL), was added sodium hydroxide (5 g, 125 mmol) as a solution in water (15 mL) followed by tri n-butyl benzyl ammonium chloride (25 mg). The two-phase solution was stirred at about 0° C. and di t-butylcarbonate (1.25 g, 5.7 mmol) was added in one portion. The mixture was stirred for about 1 h at about 0° C., the toluene layer was separated and the aqueous layer was extracted with ethyl acetate (2×10 mL). The combined organic layers were washed with water (2×10 mL); dried (MgSO4) and concentrated under in vacuo to afford the crude product (725 mg, 96% yield). ES-MS (M+H)+ 282.0 (calc. 282.1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07439231B2 |
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| Source dataset | uspto-grants-2008_10 |
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| ORD ID | ord-57c35a9f862444f18e95c94f54a0dcec |
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| Source note | uspto-grants-2008_10 |
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