Calcium Carbonate → 2-Bromo-5-fluorobenzyl alcohol

HRID 23447

반응식

HRID 23447 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 27733492-Bromo-5-fluorobenzyl alcohol

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-1076bffe427846ac8eb8c24fef4f4f01
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852711B2

연결된 노트

불러오는 중…