Calcium Carbonate → HCID 22648003、化合物
反応式
Br[CH2:2][C:3]1[C:8]([Br:9])=[CH:7][C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:4]=1[Br:13].C([O-])([O-])=[O:15].[Ca+2]>O1CCOCC1.O>[OH:15][CH2:2][C:3]1[C:8]([Br:9])=[CH:7][C:6]([N+:10]([O-:12])=[O:11])=[CH:5][C:4]=1[Br:13]参加物
5
実験手順
A mixture of 1-bromomethyl-2,6-dibromo-4-nitrobenzene (4.45 g, 1 eq.) and CaCO3 (5.7 g, 5 eq.) in 1,4-dioxane (20 mL) and water (20 mL) was heated to and maintained at reflux overnight. The mixture was cooled, poured into water and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrousmgSO4, filtered and concentrated. The product was purified by silica gel chromatography (eluted with 4:1 hexanes:ethyl acetate) to give 1-Hydroxymethyl-2,6-dibromo-4-nitrobenzene. 1H NMR (500 MHz, CDCl3) δ CHCl3: 2.28 (1H, broad t), 5.05(2H, m), 8.397(2H, s).
後処理
- temperaturewas heated to and
- temperaturemaintained
- temperatureat reflux overnight
- temperatureThe mixture was cooled
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- customdried over anhydrousmgSO4,
- filtrationfiltered
- concentrationconcentrated
- customThe product was purified by silica gel chromatography (eluted with 4:1 hexanes:ethyl acetate)
出典と根拠
- ORDレコード
- ord-0b20ce1b46394d309386f5b920be8c26
- 出典データセット
- uspto-grants-2004_10
- 特許番号
- US06809199B2
反応ノート
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