HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1481435Generated: November 1, 2026
Potassium Phosphate, Tribasic → HCID 59368312, compound
https://huagongshe.com/reaction/1481435
Participants
| Role | Name | HCID | Charge |
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| Reactant | Potassium Phosphate, Tribasic | HCID 62657 | — |
| Reactant | Morpholine, 4-(chloroacetyl)- | HCID 74040 | — |
| Reactant | L-Proline | HCID 145742 | — |
| Reactant | 9-Chloro-3-methyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole | HCID 68558507 | — |
| Catalyst | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59368312 | HCID 59368312 | 13.5% |
Reaction Steps
The title compound was prepared by following general procedure 7. 9-Chloro-3-methyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole (100 mg, 0.43 mmol), was taken into DMF. To the above solution CuI (8 mg, 0.043 mmol), L-proline (9 mg, 0.086 mmol), K3PO4 (183 mg, 0.86 mmol) were added and stirred for 10 min. at RT. 2-Chloro-1-morpholinoethanone (84 mg, 0.51 mmol) was added dropwise. The reaction mixture was heated at 90° C. for 12 h. After completion of reaction, the reaction mixture was filtered through Celite. DMF was evaporated under reduced pressure and then extracted with ethyl acetate. The organic layer was dried over Na2SO4, and concentrated under reduced pressure to obtain 21 mg of 2-(9-chloro-3-methyl-2,3,4,5-tetrahydroazepino[4,5-b]indol-6(1H)-yl)-1-morpholinoethanone as the TFA salt after purification by reverse-phase chromatography (C-18, 500 mm×50 mm, Mobile Phase A=0.05% TFA in water, B=0.05% TFA in acetonitrile, Gradient: 10% B to 80% B in 30 min., injection vol. 5 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09409910B2 |
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| Source dataset | uspto-grants-2016_08 |
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| ORD ID | ord-75f90153fa094bc689088b5204a79474 |
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| Source note | uspto-grants-2016_08 |
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