Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Acetone | HCID 180 | — |
| Reactant | Temozolomide hydrochloride | HCID 11658676 | — |
| Solvent | Water | HCID 962 | — |
| Product | Temozolomide | HCID 5394 | 88% |
Reaction Steps
A 500 ml reaction vessel equipped with a magnetic stirrer and a reflux condenser was charged with Temozolomide hydrochloride (7.2 gram, 0.031 mol), acetone (85 ml), acetic acid (1.8 ml) and water (90 ml). The reaction mixture was heated to reflux and stirring was maintained at this temperature for about 10 minutes. The reaction mixture was filtered at elevated temperature and then cooled to 5° C. for about half an hour to enable crystallization. The crystals thus obtained were collected and washed with water (2×20 ml) and cold acetone (20 ml). The crystals were dried at 40° C. in vacuum to obtain 5.3 grams (0.027 mol) of free Temozolomide base (88% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07612202B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-a7912e26033a4dc29f3d6e1fb51d3084 |
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| Source note | uspto-grants-2009_11 |
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