HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1630631Generated: November 1, 2026
HCID 68283812, compound → HCID 68284543, compound
https://huagongshe.com/reaction/1630631
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 68283812 | HCID 68283812 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68284543 | HCID 68284543 | 108% |
Reaction Steps
4-(2,8-Dimethyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-3-pyridin-4-yl-butyricacidmethylester (1.5 g, 3.9 mmol) was dissolved in THF (50 mL) and cooled to −78° C., tert-butyl lithium (16% in pentane) (6 mL, 15.13 mmol) was added dropwise under nitrogen. The reaction mixture was stirred at −78° C. for 90 min. After complete consumption of starting material, the reaction mixture was quenched with ammonium chloride solution and the reaction mixture was allowed to come to RT and extracted with EtOAc (3×100 mL). The combined organic layer was dried over anhydrous sodium sulfate and concentrated to obtain 1.7 g of crude 6-(2,8-dimethyl-1,2,3,4-tetrahydro-pyrido[4,3-b]indol-5-yl)-2,2-dimethyl-5-pyridin-4-yl-hexan-3-one. 1H NMR (CDCl3, freebase) δ (ppm): 8.41 (d, 2H), 7.31 (d, 1H), 7.19 (s, 1H), 7.1 (d, 1H), 6.93 (d, 2H), 4.25 (dd, 1H), 3.9 (t, 2H), 3.8 (m, 1H), 3.67 (dd, 1H), 2.87 (m, 3H), 2.71 (m, 2H), 2.51 (s, 3H), 2.42 (s, 3H), 2.1 (m, 1H), 1.21 s (9H). Separation by chiral HPLC provides enantiomers II-222a-b.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08791132B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-45ee13a59eb74519b541458ac0949be1 |
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| Source note | uspto-grants-2014_07 |
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