Dichloromethane → HCID 19047584、化合物

HRID 742454ノート

反応式

HRID 742454 の反応式
[O:1]1[CH:5]=[CH:4][C:3]([C:6](=O)[CH2:7]C)=[CH:2]1.[C:10](=[O:13])([O-])[O-].[K+].[K+].[CH2:16](Cl)Cl>O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[O:1]1[CH:5]=[CH:4][C:3]([C:6]([O:13][CH2:10][CH3:16])=[CH2:7])=[CH:2]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 150538531-(3-Furanyl)-1-propanone

生成物 1

HCID 19047584HCID 19047584、化合物収率 29%

試薬・触媒・溶媒 1

HCID 521998p-Toluenesulfonic acid monohydrate触媒

実験手順

To a stirring mixture of 1-(3-furyl)-1-propanone (6.75 g, 0.0612 mol) in 150 mL of methylene chloride was added TEOF (13.2 mL, 0.079 mol) with stirring followed by 100 mg of p-toluenesulfonic acid monohydrate and the resulting mixture was stirred for 126 h. Potassium carbonate (2 g) was added to the above reaction mixture, stirred for 10 min, filtered, and concentrated in vacuo. The residue was distilled (35 mm, 82°-85° C.) to afford 2.5 g (29%) of 1-(3-furyl)-1-ethoxy-ethylene (Formula III: R3 =R4 =H; R5 =CH3CH2O; R6 =3-furanyl), as a clear oil.

後処理

  1. additionwas added TEOF (13.2 mL, 0.079 mol)
  2. stirringthe resulting mixture was stirred for 126 h
  3. stirringstirred for 10 min
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. distillationThe residue was distilled (35 mm, 82°-85° C.)

出典と根拠

ORDレコード
ord-751fad5a61b14a0b9cac4ddde9d5ef36
出典データセット
uspto-grants-1996_09
特許番号
US05554620

反応ノート

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