p-Toluenesulfonic acid monohydrate → 2-(5-Bromoindane-1-ylidene)-1,3-dithiane

HRID 2046552

반응식

HRID 2046552 반응식
[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7]([CH:12]1[S:17][CH2:16][CH2:15][CH2:14][S:13]1)(O)[CH2:6][CH2:5]2.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[Br:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[C:12]1[S:13][CH2:14][CH2:15][CH2:16][S:17]1)[CH2:6][CH2:5]2

참가 물질

4

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 574194845-bromo-1-(1,3-dithian-2-yl)-2,3-dihydro-1H-inden-1-ol

생성물 1

HCID 574194852-(5-Bromoindane-1-ylidene)-1,3-dithiane

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

A mixture of (rac)-5-bromo-1-[1,3]dithian-2-yl-indan-1-ol (2.15 g, 6.49 mmol) and p-toluenesulfonic acid monohydrate (309 mg, 1.62 mmol) in benzene (30 ml) was heated to reflux for 2 h using a Dean-Stark trap to remove water. The brown solution was allowed to cool to room temperature and was diluted with sat. NaHCO3 solution. The layers were separated and the organic layer was washed with brine, dried with Na2SO4 and evaporated. The title compound was obtained as brown gum (2.024 g, 99%) and was used without purification for the next reaction step.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 2 h
  3. customto remove water
  4. additionwas diluted with sat. NaHCO3 solution
  5. customThe layers were separated
  6. washthe organic layer was washed with brine
  7. dry with materialdried with Na2SO4
  8. customevaporated

출처 및 근거

ORD 기록
ord-074c5ef97fa1482094f2dbc5e672e221
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592426B2

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