Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 117857366 | HCID 117857366 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 117856778 | HCID 117856778 | 98% |
Reaction Steps
A solution of 7-methyl-5-(pyridin-4-yl)-3-(2,2,2-trifluoroethyl)-3H-pyrrolo[2,3-d]pyrimidin-4(7H)-one (130 mg, 0.422 mmol) in DMF (6 ml) was cooled to 0° C. Bromine (0.026 ml, 0.506 mmol) was added dropwise. The resulting mixture was stirred at 0° C. for 60 min. The reaction mixture was partitioned between ethyl acetate (40 ml) and a mixture of aqueous (3:1:4, water, sodium bicarbonate solution and 20% w/w sodium thiosulfate solution, 40 ml). The organic phase was separated and washed with water (3×30 ml), brine and concentrated to give the title compound (160 mg, 98%). LCMS RT=0.72 min, [M+H+(79Br)]=387.0, [M+H+(81Br)]=389.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09156853B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-92300415451b478a870dc525fda0b27a |
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| Source note | uspto-grants-2015_10 |
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