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Water → 5724-03-8

HRID 2259436
ノート
印刷プレビュー

反応式

HRID 2259436 の反応式
[CH:1]([Mg]Cl)=[CH2:2].[F:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]=[O:11])=[CH:8][CH:7]=1.O>O1CCCC1>[F:5][C:6]1[CH:13]=[CH:12][C:9]([CH:10]([OH:11])[CH:1]=[CH2:2])=[CH:8][CH:7]=1
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 962WaterHCID 680234-FluorobenzaldehydeHCID 178461836HCID 178461836、化合物

生成物 1

HCID 150949505724-03-8収率 99%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1,550 ml (2.0 mol) of a 1.29 M solution of vinylmagnesium chloride in tetrahydrofuran were introduced into a 4 l stirred flask under nitrogen. Subsequently, while stirring under nitrogen at 30°-35° C., a solution of 222.0 g (1,764 mol) of 4-fluorobenzaldehyde in 2,000 ml of tetrahydrofuran was added over the course of 30 min, cooling the reaction mixture with ice. The mixture was then stirred at room temperature under nitrogen for 2.5 h. Subsequently, while stirring and cooling with ice, 180 ml of water were added, the mixture was filtered with suction, and the residue from the filter was washed 3x with 150 ml of tetrahydrofuran. The filtrates were combined, dried with sodium sulfate and concentrated. 265.7 g (99%) of product were obtained in the form of a yellow-brown oil.

後処理

  1. stirringSubsequently, while stirring under nitrogen at 30°-35° C.
  2. temperaturecooling the reaction mixture with ice
  3. stirringThe mixture was then stirred at room temperature under nitrogen for 2.5 h
  4. stirringSubsequently, while stirring
  5. additionwere added
  6. filtrationthe mixture was filtered with suction
  7. washthe residue from the filter was washed 3x with 150 ml of tetrahydrofuran
  8. dry with materialdried with sodium sulfate
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-a3d05ef045d442d9a5790a55a87d85b1
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05473080

反応ノート

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