Tetrahydrofuran → HCID 57925986、化合物

HRID 1013455ノート

反応式

HRID 1013455 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([P:9](Cl)(Cl)=[O:10])=[CH:5][CH:4]=1.[CH2:13]1[CH2:17]OCC1.[CH:18]([Mg]Br)=[CH2:19]>CCOCC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([P:9](=[O:10])([CH:18]=[CH2:19])[CH:13]=[CH2:17])=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 2167114-Methoxyphenylphosphonic DichlorideHCID 178418507HCID 178418507、化合物

生成物 1

HCID 57925986HCID 57925986、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

(4-Methoxyphenyl)phosphonic dichloride (2.00 g, 8.89 mmol) was made 0.1 M in 1:1 THF:ether and stirred at −78° C. To this stirring solution vinyl magnesium bromide (17.8 mL, 17.78 mmol, 1M in THF) was added dropwise. The mixture was stirred for 1 h, then quenched with 2M aq. HCl and extracted with DCM (3×). The combined organic extracts were washed with brine, dried (MgSO4) and concentrated to afford the requisite product. MS: cal'd 209 (MH+), exp 209 (MH+)

後処理

  1. customquenched with 2M aq. HCl
  2. extractionextracted with DCM (3×)
  3. washThe combined organic extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customto afford the requisite product

出典と根拠

ORDレコード
ord-1916c2b9b7744bfc891888a625c187c5
出典データセット
uspto-grants-2011_07
特許番号
US07981874B2

反応ノート

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