Chloroform → Thiophene, 3-(bromomethyl)-2,5-dihydro-, 1,1-dioxide

HRID 1462857

반응식

HRID 1462857 반응식
[CH3:1][C:2]1[CH2:3][S:4]([CH2:7][CH:8]=1)(=[O:6])=[O:5].[Br:9]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(Cl)(Cl)Cl>CCOCC>[Br:9][CH2:1][C:2]1[CH2:3][S:4]([CH2:7][CH:8]=1)(=[O:6])=[O:5]

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 70941Thiophene, 2,5-dihydro-3-methyl-, 1,1-dioxide

생성물 1

HCID 712958Thiophene, 3-(bromomethyl)-2,5-dihydro-, 1,1-dioxide수율 34.2%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

In a reaction vessel, 21.0 gms (0.1591 moles) 3-methyl sulfolene, 28.32 gms (0.1591 moles) N-bromo succinimide, 1.9 gms (0.0008 moles) benzoyl peroxide and 250 ml chlorform were combined. The resulting mixture was heated to reflux and then refluxed for 20 hours. The reaction mixture was cooled to 0° C. and then filtered to remove the succinimide. The filtrate was stripped until only a small amount of solvent remained. The remaining solids were removed by filtration, and the remainder of the solvent was stripped to give an orange oil. Ether was added to the oil. After a few minutes, the solids crystallized. Filtration and drying yielded 11.5 gms of the product. The NMR and IR spectra confirmed the structure.

후처리

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. temperaturerefluxed for 20 hours
  4. filtrationfiltered
  5. customto remove the succinimide
  6. customThe remaining solids were removed by filtration
  7. customto give an orange oil
  8. waitAfter a few minutes
  9. customthe solids crystallized
  10. filtrationFiltration
  11. customdrying

출처 및 근거

ORD 기록
ord-4ee0407e9047430eacd01aa33f279a11
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04461764

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