Phenacyl bromide → 1,4-Dithiin, 2,3-dihydro-5-phenyl-

HRID 839388ノート

反応式

HRID 839388 の反応式
[CH2:1](Br)[C:2]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=O.[CH2:11]([SH:14])[CH2:12][SH:13]>C1C=CC=CC=1>[C:4]1([C:2]2[S:13][CH2:12][CH2:11][S:14][CH:1]=2)[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

参加物

4

反応物 2

HCID 6259Phenacyl bromideHCID 109021,2-Ethanedithiol

生成物 1

HCID 6065711,4-Dithiin, 2,3-dihydro-5-phenyl-

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

By following substantially the procedure of Example 4, Step A, phenacyl bromide (95.0 g.) and ethane-1,2-dithiol (40.0 ml.) in benzene (500 ml.) is allowed to stand for 2 days at room temperature (until gas chromatography indicates the absence of starting material). Solid by-product is removed by filtration and the filtrate is washed with aqueous sodium bicarbonate solution and water. The product solution is dried over anhydrous sodium sulfate. Solvent is removed by distillation and the residual oil is distilled at reduced pressure to afford 2-phenyl-5,6-dihydro-1,4-dithiin (47.2 g.; b.p. 140°-150° C./0.25 mm.). The product solidifies on standing and is recrystallized from methanol (m.p. 58.0°-59.0° C.).

後処理

  1. customSolid by-product is removed by filtration
  2. washthe filtrate is washed with aqueous sodium bicarbonate solution and water
  3. dry with materialThe product solution is dried over anhydrous sodium sulfate
  4. customSolvent is removed by distillation
  5. distillationthe residual oil is distilled at reduced pressure

出典と根拠

ORDレコード
ord-1c3baa47e6344938baa17c58475b81cb
出典データセット
uspto-grants-1978_06
特許番号
US04094988

反応ノート

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