Carbon tetrabromide → HCID 21476913、化合物

HRID 2293583ノート

反応式

HRID 2293583 の反応式
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]

参加物

5

反応物 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 21476897HCID 21476897、化合物

生成物 1

HCID 21476913HCID 21476913、化合物収率 94.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1c48d9c1d6c946cda3fe851aca13b0e9
出典データセット
uspto-grants-1997_11
特許番号
US05686478

反応ノート

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