反応式
[CH3:1][C:2]([C:4]([CH3:6])=[CH2:5])=[CH2:3].[CH2:7]([OH:13])[CH2:8][CH2:9][CH2:10][C:11]#[CH:12]>[Co](Br)Br.[I-].[Zn+2].[I-].[Zn].C1(P(C2C=CC=CC=2)CCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1COCC1>[CH3:3][C:2]1[CH2:1][CH:12]=[C:11]([CH2:10][CH2:9][CH2:8][CH2:7][OH:13])[CH2:5][C:4]=1[CH3:6]参加物
反応条件
- 温度
- 70 °C
実験手順
800 mg (2.00 mmol) of 1,2-bis(diphenylphosphino)ethane, 437 mg (2.00 mmol) of cobalt bromide, 1.28 g (4.00 mmol) of zinc iodide, and 260 mg (4.00 mmol) of zinc were added to 40 ml of THF, and the solution was stirred for 15 minutes at 70° C. The solution was cooled to room temperature, and 9.86 g (120 mmol) of 2,3-dimethyl-1,3-butadiene was added thereto. Subsequently, 9.8 g (100 mmol) of 5-hexyn-1-ol was slowly added dropwise to the mixture in a water bath. The resulting mixture was stirred for one hour at 35° C., and then the solvent was distilled off under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (hexane/ethyl acetate=3/1), and thus 11.5 g of the title compound alcohol was obtained as a colorless oil. Yield 63.4%.
後処理
- temperatureThe solution was cooled to room temperature
- stirringThe resulting mixture was stirred for one hour at 35° C.
- distillationthe solvent was distilled off under reduced pressure
- customThe residue thus obtained
- customwas purified by silica gel column chromatography (hexane/ethyl acetate=3/1)
出典と根拠
- ORDレコード
- ord-cdea10847ceb4f538304e63fca57255b
- 出典データセット
- uspto-grants-2015_12
- 特許番号
- US09217005B2
関連ノート
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