Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | 4-Chloro-2-(2-chloro-acetylamino)-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid methyl ester | HCID 11633641 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 131728504 | HCID 131728504 | — |
Reaction Steps
Morpholine (0.235 mL, 2.7 mmol) was added to a solution of Example 133 (0.6 g, 1.3 mmol) in DMF (8 mL). The reaction mixture was stirred at 120° C. for 4 h, concentrated, treated with water and the solid that precipitated was filtered, washed with water and purified using flash chromatography (silica gel, 1% methanol/chloroform) to obtain the title compound. Yield: 0.57 g, (85%); 1H NMR (DMSO-d6): δ 2.7 (s, 3H, CH3), 3.2 (s, 2H, CH2), 3.7 (t, 4H, 2CH2), 3.9 (s, 2H, CH2), 4.28 (s, 2H, CH2), 5.35 (s, 2H, CH2), 7.82 (d, 1H, Ar), 8.0 (s, 1H, Ar), 8.12 (s, 1H, Ar), 8.2 (s, 1H, Ar); MS: m/e (CI+) 495 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07834001B2 |
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| Source dataset | uspto-grants-2010_11 |
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| ORD ID | ord-bd6e398cc5734e049f16e38471aaa203 |
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| Source note | uspto-grants-2010_11 |
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