Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1032265-57-8 | HCID 56935577 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66558501 | HCID 66558501 | 83% |
Reaction Steps
4.25 g (10 mmol) (Z)—N-[2-(diethylamino)ethyl]-2-methyl-7-(1,2-dihydro-5-fluoro-2-oxo-3H-indol-3-ylidene)-4,5,6,7-tetrahydro-1H-indol-3-carboxamide was added to a mixture of 250 ml acetonitrile and 50 ml dichloromethane. The mixture was treated under ultrasonic sound to uniform dispersion. 1.11 g (11.5 mmol) methanesulfonic acid was added and the solution was heated to reflux with stirring under nitrogen atmosphere. After reaction for 1 h, the resulting solution was filtered while being hot, and the filtrate was concentrated at reduced pressure to dryness, added to 30 ml anhydrous ethanol and treated under ultrasonic sound to uniform dispersion. Then the solution was filtered, and the filter cake was dried at 40° C. under vacuum, to give the title compound as orange solid (4.33 g, 8.3 mmol, yield 83%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09018242B2 |
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| Source dataset | uspto-grants-2015_04 |
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| ORD ID | ord-fb90f5f76f0a4a39a875ac7436aeab1a |
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| Source note | uspto-grants-2015_04 |
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