Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trimethyl phosphite | HCID 8472 | — |
| Reactant | Carbon tetrabromide | HCID 11205 | — |
| Reactant | HCID 59837290 | HCID 59837290 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 59837324 | HCID 59837324 | — |
Reaction Steps
To a methylene chloride solution (2 mL) containing the compound of Example 219 (860 mg), carbon tetrabromide (533 mg) and pyridine (2 mL), trimethyl phosphite (0.19 mL) was added while the mixture was stirred at 0° C. and the mixture was stirred for 5 hours until room temperature. Subsequently, water was added and the mixture was extracted with ethyl acetate. The extract was washed sequentially with water and a saturated aqueous solution of sodium chloride. The organic phase was then dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was purified on a silica gel column chromatography (hexane:ethyl acetate=1:1) to obtain the desired product as a colorless oil (830 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07759326B2 |
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| Source dataset | uspto-grants-2010_07 |
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| ORD ID | ord-3c20a78fa3c14d0893c8348ed1dd258f |
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| Source note | uspto-grants-2010_07 |
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