HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 89155066, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70976451 | HCID 70976451 | — |
| Catalyst | Titanium(2+);dichloride | HCID 10290777 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 89155066 | HCID 89155066 | 116.9% |
Reaction Steps
A solution of titanous chloride (about 15%) in about 10% hydrochloric acid (MERCK (MDA) INCL SCHUCHARDT, 71.5 mL) was added to a stirred solution of 1-fluoro-2-[(methylsulfonyl)methyl]-4-nitrobenzene (1.61 g) in THF (80 mL) at room temperature and stirred for 16 hours. By adding 1N sodium hydroxide solution the pH value of the reaction mixture was raised to 10 before it was extracted with ethyl acetate (2×). The combined organic phases were washed with brine, dried over sodium sulfate and concentrated to give the crude title compound (1.64 g) which crystallized from diethylether/Ethyl acetate (1.16 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08916557B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-d594f12053994633a5240dbbf9c9d4c1 |
| Source note | uspto-grants-2014_12 |