Carbon tetrabromide → HCID 21476913, 화합물

HRID 2293583노트

반응식

HRID 2293583 반응식
O[CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:36]>C(Cl)Cl>[Br:36][CH2:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15]

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 21476897HCID 21476897, 화합물

생성물 1

HCID 21476913HCID 21476913, 화합물수율 94.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a magnetically stirred solution of 0.405 g (1.94 mmol) of the product of Step D dissolved in 5.0 mL of methylene chloride was added 0.638 g (2.43 mmol) of triphenylphosphine followed by 0.806 g (2.43 mmol) of carbon tetrabromide at room temperature. The reaction mixture was stirred for 30 minutes at room temperature, then the magnetic stir bar was removed and the methylene chloride was evaporated in vacuo. The residue was purified on a silica gel flash chromatography column eluted with 10% EtOAc-hexane, and evaporation of the purified fractions and solvent removal in vacuo afforded 0.496 g (94%) of the title compound.

후처리

  1. customthe magnetic stir bar was removed
  2. customthe methylene chloride was evaporated in vacuo
  3. customThe residue was purified on a silica gel flash chromatography column
  4. washeluted with 10% EtOAc-hexane, and evaporation of the purified fractions and solvent removal in vacuo

출처 및 근거

ORD 기록
ord-1c48d9c1d6c946cda3fe851aca13b0e9
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05686478

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