HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 58707330, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4-Difluoro-1-(methylsulfonyl)benzene | HCID 2758336 | — |
| Reactant | 6-Chloro-3,4-dihydro-2H-1-benzopyran-4-amine--hydrogen chloride (1/1) | HCID 52988847 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 58707330 | HCID 58707330 | 16.1% |
Reaction Steps
A solution of 6-chlorochroman-4-amine hydrochloride (551.0 mg, 2.50 mmol), 2,4-difluoro-1-(methylsulfonyl)benzene (496.0 mg, 2.50 mmol) and diisopropylethylamine (1.29 g, 10.0 mmol) in N,N-dimethylformamide (10 mL) was stirred at 110° C. for 16 h. The reaction was cooled to room temperature, poured over water and extracted with diethyl ether. The solvent was concentrated in vacuo and the residue was purified by silica chromatography (20% ethyl acetate in hexanes) to yield 143.0 mg (16%) of the desired product: 1H NMR (400 MHz, CDCl3) δ 7.82 (dd, 1H), 7.19 (m, 2H), 6.83 (d, 1H), 6.57 (m, 2H), 4.60 (m, 1H), 4.30 (m, 1H), 4.28 (m, 1H), 3.01 (s, 3H), 2.19 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07968538B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-50f4b89d4e02466f9370a377bcb9f75b |
| Source note | uspto-grants-2011_06 |