HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2401673Generated: October 30, 2026
HCID 59234237, compound → HCID 59234229, compound
https://huagongshe.com/reaction/2401673
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | HCID 59234237 | HCID 59234237 | — |
| Reactant | HCID 178419730 | HCID 178419730 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59234229 | HCID 59234229 | 64% |
Reaction Steps
To a solution of intermediate 5 (10.4 g, 54.67 mmol) in DMF (250 ml) was added phosphorus(III) oxybromide (31.3 g, 109.3 mmol) and the mixture was heated at 110° C. for 1.5 hours. After cooling in an ice bath the solution was partitioned between water and EtOAc. After three extractions with EtOAc the combined organic fractions were washed with brine, dried over MgSO4 and the solvent evaporated in vacuo. The crude product was purified by column chromatography (silica gel; DCM as eluent). The desired fractions were collected and evaporated in vacuo to yield intermediate 8 (8.83 g, 64%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08796311B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-3787de649d1e4ad7acd72bf752f4bebb |
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| Source note | uspto-grants-2014_08 |
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