HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 2-Methyl-5-(4-(2-nitro-ethyl)-benzyl)-furan
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 2-Methyl-5-(4-((E)-2-nitro-vinyl)-benzyl)-furan | HCID 59255436 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Methyl-5-(4-(2-nitro-ethyl)-benzyl)-furan | HCID 59255527 | 77% |
Reaction Steps
To a mixture of 2-methyl-5-(4-((E)-2-nitro-vinyl)-benzyl)-furan (120 mg) described in Manufacturing Example 46-1-4, acetic acid (0.2 mL) and dimethyl sulfoxide (3.4 mL) was added sodium borohydride (29 mg, 0.77 mmol) at room temperature while cooling appropriately, which was stirred for 20 minutes at room temperature. Water was added to the reaction mixture, which was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and was concentrated under a reduced pressure. The residue was purified by neutral silica gel column chromatography (ethyl acetate:heptane=1:5) to obtain the title compound (90 mg, 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07691882B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-c2b2ba30ed444ec98e3d7e4b6c223f27 |
| Source note | uspto-grants-2010_04 |