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

HRID 839388노트

반응식

HRID 839388 반응식
[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

참가 물질

4

반응물 2

HCID 6259Phenacyl bromideHCID 109021,2-Ethanedithiol

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-1c3baa47e6344938baa17c58475b81cb
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04094988

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