Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | HCID 58456641 | HCID 58456641 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178503058 | HCID 178503058 | 44% |
Reaction Steps
(6aR,9aS)-5,6a,7,8,9,9a-hexahydro-5-methyl-3-(methylthio)-2-(4-(6-fluoropyridin-2-yl)benzyl)-cyclopent[4,5]imidazo[1,2-a]pyrazolo[4,3-e]pyrimidin-4(2H)-one (25 mg, 0.054 mmol) and P4S10 (48.1 mg, 0.108 mmol) are placed in a Biotage microwave vial, and then 1.0 mL of 7N ammonia in MeOH is added. The sealed vial is heated in a Biotage microwave at 150° C. for 6 h. After solvent is removed, the residue is suspended in DMF, and then filtered. The obtained filtrate is purified by a semi-preparative HPLC to give 10.6 mg of pure product as pale yellow solids (yield: 44%). MS (ESI) m/z 449.2 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08536159B2 |
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| Source dataset | uspto-grants-2013_09 |
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| ORD ID | ord-36ad0d15757644df8a70ab716eacc39d |
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| Source note | uspto-grants-2013_09 |
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