HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → 2-(4-(2-Nitro-ethyl)-phenoxymethyl)-pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | Sodium borohydride | HCID 4311764 | — |
| Reactant | 2-(4-((E)-Nitro-vinyl)-phenoxymethyl)-pyridine | HCID 59255195 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 2-(4-(2-Nitro-ethyl)-phenoxymethyl)-pyridine | HCID 59255522 | 20% |
Reaction Steps
To a solution of 2-(4-((E)-nitro-vinyl)-phenoxymethyl)-pyridine (33.9 g, 132 mmol) described in Manufacturing Example 203-1-2 in acetic acid (34 mL) and dimethyl sulfoxide (576 mL) was added sodium borohydride (7.99 g, 211 mmol) at room temperature while cooling appropriately. This mixture was stirred for 5 hours at room temperature. This mixture was partitioned into ethyl acetate and water. The organic layer was separated, washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure, and the residue was recrystallized from heptane and ethyl acetate to obtain the title compound (6.81 g, 20%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08158657B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-ba8cab08715a4087960de195b4102333 |
| Source note | uspto-grants-2012_04 |