Participants
| Role | Name | HCID | Charge |
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| Reactant | HCID 524499 | HCID 524499 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | N-ethyl carbazole | HCID 6836 | 82% |
| Product | HCID 524499 | HCID 524499 | 17% |
Reaction Steps
70 g of 9-ethyl-1,2,3,4-tetrahydrocarbazole was charged along with 3.5 g of filtered wet catalyst obtained from above batch (2 wt % on dry basis) and 35 ml o-xylene. The content were heated under a slow current of nitrogen to achieve 200° C. liquid temperature and maintained for 15 hour to get GC conversion of 82% 9-ethyl carbazole and 17% 9-ethyl-tetrahydrocarbazole. Further, 0.3 g fresh 5%-Pd-carbon (50% moisture) was added at this stage and the reaction was maintained at 200° C. for further 6 hours to get 99% conversion. The reaction mass was then filtered to remove the catalyst and the filtrate was concentrated under reduced pressure to get 67.9 g crude product with GC purity of 98.4%. Filtered catalyst was further recycled three times by adding fresh 5% Pd-c catalyst, 10% of initial catalyst loading to achieve higher conversion.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08604219B2 |
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| Source dataset | uspto-grants-2013_12 |
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| ORD ID | ord-ad6bfffb94194cc385b473ae03886262 |
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| Source note | uspto-grants-2013_12 |
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