HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuryl chloride → 2-Chloro-4-(trifluoromethoxy)phenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | p-(Trifluoromethoxy)phenol | HCID 70015 | — |
| Product | 2-Chloro-4-(trifluoromethoxy)phenol | HCID 13044783 | 94.1% |
Reaction Steps
A solution of 4-trifluoromethoxyphenol (20 g, 0.11 mole) and sulfuryl chloride (18.20 mL, 0.22 mole) was stirred at room temperature for five hours. The excess of sulfuryl chloride was evaporated by rotary evaporator. The residue was dissolved in 50 mL of dichloromethane and washed with 50 mL of H2O. The organic layer was separated, dried over MgSO4, filtered and concentrated to yield 22 g of the product. The crude product was purified over a silica gel column using 10% ethyl acetate in hexane to yield 16.4 g of the product. 1H-NMR (DMSO, 500-MHz), δ 10.59 (s, 1H), 7.43 (d, J=2.75 Hz, 1H), 7.18 (dd, J1=2.75 Hz, J2=7.16 Hz, 1H), 7.03 (d, J=7.16 Hz, 1H). MS (electro-spray) [M−H] 211.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07256218B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-989e6bbea2584273aa3c15c04c2f5990 |
| Source note | uspto-grants-2007_08 |