HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-(Trifluoromethyl)aniline → 2-Iodo-4-(trifluoromethyl)aniline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-(Trifluoromethyl)aniline | HCID 9964 | — |
| Reactant | Iodine chloride | HCID 24640 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2-Iodo-4-(trifluoromethyl)aniline | HCID 2783322 | 70.6% |
Reaction Steps
Preparation B5, Step 1: To a solution of 4-(trifluoromethyl)benzenamine (10.0 g, 0.0617 mol) in dry methanol (200 ml) was added iodine monochloride (10.49 g, 0.148 mol) in dry MDC (40 ml) at RT slowly. Reaction mixture was stirred at RT over night. The reaction mixture was concentrated, water was added and extracted with ethyl acetate (2×100 ml). The organic layer was washed with water, brine (2×50 ml), dried over Na2SO4 and concentrated. The crude product was purified by column chromatography using 6% ethyl acetate in pet-ether to get 2-iodo-4-(trifluoromethyl)benzenamine (12.5 g, 70%) as pale yellow liquid. 1H NMR (400 MHz, CDCl3) δ 4.42 (bs, 2H), 6.75 (d, 1H), 7.38 (d, 1H), 7.87 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07163937B2 |
| Source dataset | uspto-grants-2007_01 |
| ORD ID | ord-9a30700b78d44c3da632cf65f0f33fd6 |
| Source note | uspto-grants-2007_01 |