Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiomorpholine | HCID 67164 | — |
| Reactant | HCID 10243527 | HCID 10243527 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67042704 | HCID 67042704 | — |
Reaction Steps
The process is performed as in Example 75, starting with 500 mg of 2-chloro-N-(6-chloro-1H-indazol-3-yl)acetamide, 15 cm3 of acetonitrile and 0.62 cm3 of thiomorpholine. The reaction medium is refluxed for 2 hours, the precipitate formed is filtered off and the filtrate is concentrated to dryness under reduced pressure (2 kPa; 50° C.); the crude product obtained is purified by chromatography under an argon pressure of 50 kPa, on a column of silica gel (particle size 40-60 μm; diameter 2.5 cm), eluting with a cyclohexane/ethyl acetate mixture (50/50 by volume). The fractions containing the expected product are combined, evaporated under reduced pressure (2 kPa; 50° C.) and dried (90 Pa; 45° C.) to give 560 mg of N-(6-chloro-1H-indazol-3-yl)thiomorpholine-4-acetamide in the form of a pale yellow foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06949579B2 |
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| Source dataset | uspto-grants-2005_09 |
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| ORD ID | ord-75a212d66b9c4713b13ead7b0216cbc3 |
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| Source note | uspto-grants-2005_09 |
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