Calcium Carbonate → 2-Bromo-5-fluorobenzyl alcohol

HRID 23447

反応式

HRID 23447 の反応式
[Br:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH2:4]Br.C([O-])([O-])=[O:12].[Ca+2]>O1CCOCC1.O>[Br:1][C:2]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][C:3]=1[CH2:4][OH:12]

参加物

5

反応物 2

HCID 10112Calcium CarbonateHCID 5179721-Bromo-2-(bromomethyl)-4-fluorobenzene

生成物 1

HCID 27733492-Bromo-5-fluorobenzyl alcohol

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

2-Bromo-5-fluorobenzylbromide (2.0 g, 7.46 mmol) was dissolved in dioxane (25 mL) and H2O (25 mL), and CaCO3 (3.84 g, 38.39 mmol) was added. The mixture was heated to reflux overnight. The solution was concentrated, and the residue was partitioned between H2O and CH2Cl2. The organic phase was washed with 1N HCl and brine, dried (MgSO4), filtered, and concentrated to afford the title compound. 1H NMR (CDCl3): δ 2.00 (t, 1H), 4.72 (d, 2H), 6.85-6.92 (m, 1H), 7.26 (dd, 1H), 7.48 (dd, 1H).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux overnight
  3. concentrationThe solution was concentrated
  4. customthe residue was partitioned between H2O and CH2Cl2
  5. washThe organic phase was washed with 1N HCl and brine
  6. dry with materialdried (MgSO4)
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-1076bffe427846ac8eb8c24fef4f4f01
出典データセット
uspto-grants-2005_02
特許番号
US06852711B2

関連ノート

読み込み中…