Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trifluoroacetic anhydride | HCID 9845 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | 1-Azatricyclo[6.3.1.0,4,12]dodeca-2,4,6,8(12)-tetraene | HCID 15645629 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | Lilolidine | HCID 120264 | 98.5% |
Reaction Steps
A solution of 5,6-dihydro-4H-pyrrolo[3,2,1-ij]quinoline (4.0 g, 25.5 mmol) in methanol (100 ml) was treated with sodium cyanoborohydride (1.5 g, 23.9 mmol) then cooled to 0° C. Trifluoroacetic anhydride (15 ml) was added dropwise over 15 minutes, then the reaction was allowed to warm to room temperature and stirred for a further 2 hours. The reaction was basified with 5M aqueous potassium hydroxide then diluted with water (500 ml). The mixture was extracted with dichloromethane (3×100 ml) and the combined organic extracts were dried with anhydrous sodium sulfate and evaporated to dryness to obtain 1,2,5,6-tetrahydro-4H-pyrrolo[3,2,1-ij]quinoline as a colorless oil (4.0 g) which was used without further purification. LCMS: 160 [M+H].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08513292B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-d02f17d1a1ac4afbb9529876aead0dbe |
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| Source note | uspto-grants-2013_08 |
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