Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diiodomethane | HCID 6346 | — |
| Reactant | Isoamyl Nitrite | HCID 8053 | — |
| Reactant | HCID 71285432 | HCID 71285432 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 86705365 | HCID 86705365 | — |
Reaction Steps
1.500 g (3.35 mmol) of 4-amino-2-[8-(2-fluorobenzyl)imidazo[1,5-a]pyrimidin-6-yl]-5,5-dimethyl-5,7-dihydro-6H-pyrrolo[2,3-d]pyrimidin-6-one was suspended in 6.00 ml (44.56 mmol) of isopentyl nitrite and 4.00 ml (49.66 mmol) of diiodomethane and it was stirred for 2d at 85° C. 4.00 ml isopentyl nitrite and 5 ml NMP were added and the solution was stirred for 4 h at 85° C. The mixture was concentrated by evaporation in the rotary evaporator except the NMP and was purified by preparative HPLC (eluent: acetonitrile/water with 0.1% formic acid, gradient 20:80→100:0). 928 mg (purity 69%, 37% of theor.) of the target compound was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08859569B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-7ad6afdde597467190141690b5671b1f |
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| Source note | uspto-grants-2014_10 |
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