Benzene → 2-(4-Bromothiophen-2-yl)-1,3-dioxolane

HRID 2081756ノート

反応式

HRID 2081756 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:7]=[O:8])[S:5][CH:6]=1.C1(C)C=CC(S(O)(=O)=[O:16])=CC=1.[CH:20]1[CH:25]=CC=CC=1>>[Br:1][C:2]1[CH:3]=[C:4]([CH:7]2[O:16][CH2:20][CH2:25][O:8]2)[S:5][CH:6]=1

参加物

4

反応物 3

HCID 241BenzeneHCID 6101p-Toluenesulfonic acidHCID 877924-Bromothiophene-2-carbaldehyde

生成物 1

HCID 38572552-(4-Bromothiophen-2-yl)-1,3-dioxolane収率 72%

実験手順

In a 100 mL roundbottom flask equipped with a dean stark trap and a reflux condenser, 4-bromothiophene-2-carboxaldehyde (25 g, 131 mMol) and a catalytic amount of p-toluenesulfonic acid were dissolved in benzene (50 mL). The mixture was heated to reflux overnight. The reaction was cooled, washed with sat'd sodium bicarbonate, water, dried (MgSO4) and concentrated. Purification by fractional distillation (80°-90° C., 0.5 mm Hg) afforded 24.23 g (72%) of the desired dioxolane as a clear liquid.

後処理

  1. customIn a 100 mL roundbottom flask equipped with a dean stark trap and a reflux condenser
  2. temperatureThe mixture was heated
  3. temperatureto reflux overnight
  4. temperatureThe reaction was cooled
  5. washwashed with sat'd sodium bicarbonate, water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customPurification
  9. distillationby fractional distillation (80°-90° C., 0.5 mm Hg)

出典と根拠

ORDレコード
ord-410fc2c968474776b0367118b95eccbe
出典データセット
uspto-grants-1993_02
特許番号
US05185363

反応ノート

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