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Diisopropylamine → Dichloro(diisopropylamino)borane

HRID 1595105
ノート
印刷プレビュー

反応式

HRID 1595105 の反応式
[Cl:1][B:2]([Cl:4])Cl.[CH:5]([NH:8][CH:9]([CH3:11])[CH3:10])([CH3:7])[CH3:6].C(N(CC)CC)C>C(Cl)Cl>[CH:5]([N:8]([B:2]([Cl:4])[Cl:1])[CH:9]([CH3:11])[CH3:10])([CH3:7])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7912DiisopropylamineHCID 8471TriethylamineHCID 25135Boron Trichloride

生成物 1

HCID 4139105Dichloro(diisopropylamino)borane収率 51%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a methylene chloride solution of trichloroborane (1.0 M, 100 ml, 0.10 mole) was added dropwise at −78° C. diisopropylamine (13.108 ml, 0.100 mole) over a 30 minute period. The solution was allowed to stir for 1 hour, during which a white precipitate formed. The mixture was allowed to warm to room temperature, and solvent was removed under reduced pressure. The residue was dissolved in 100 ml of dry toluene, triethylamine (13.94 ml, 0.10 mole) was added and the solution was stirred overnight at room temperature. The mixture was filtered, the residue was washed with 20 ml of toluene. Solvent was removed under reduced pressure from the combined filtrates, and the resulting oil was purified by vacuum distillation (25-28° C., 13 Pa, 0.1 mm) to give 9.2 g (51 percent) of product as a colorless liquid.

後処理

  1. customformed
  2. customsolvent was removed under reduced pressure
  3. dissolutionThe residue was dissolved in 100 ml of dry toluene
  4. stirringthe solution was stirred overnight at room temperature
  5. filtrationThe mixture was filtered
  6. washthe residue was washed with 20 ml of toluene
  7. customSolvent was removed under reduced pressure from the combined filtrates
  8. distillationthe resulting oil was purified by vacuum distillation (25-28° C., 13 Pa, 0.1 mm)

出典と根拠

ORDレコード
ord-7c389eb9f7f4450d9bc39e16b6c8e4a1
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06284905B1

反応ノート

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