p-Toluenesulfonic acid monohydrate → 4-Ethyl-7-methyl-benzo[b]thiophen-5-ol

HRID 38427노트

반응식

HRID 38427 반응식
[S:1]1[CH:5]=[CH:4][C:3]([CH:6]([CH2:13][CH3:14])[C:7](=[O:12])[CH2:8][C:9](=O)[CH3:10])=[CH:2]1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1.C(OCC)C>[CH2:13]([C:6]1[C:3]2[CH:4]=[CH:5][S:1][C:2]=2[C:9]([CH3:10])=[CH:8][C:7]=1[OH:12])[CH3:14]

참가 물질

5

반응물 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 595986385-Thiophen-3-yl-heptane-2,4-dione

생성물 1

HCID 595987024-Ethyl-7-methyl-benzo[b]thiophen-5-ol

시약·촉매·용매 2

HCID 241Benzene용매HCID 3283Diethyl Ether용매

실험 절차

5-Thiophen-3-yl-heptane-2,4-dione (410 mg, 2 mmol) was dissolved in 15 ml benzene, and p-toluene sulfonic acid monohydrate (408 mg, 2 mmol) was added. The reaction mixture was heated to reflux for 30 min, cooled, diluted with diethy ether, washed with saturated sodium bicarbonate, water, brine, and dried over magnesium sulfate. Concentration in vacuo 370 mg of 4-Ethyl-7-methyl-benzo[b]thiophen-5-ol, 98%, as a white solid.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 30 min
  3. temperaturecooled
  4. washwashed with saturated sodium bicarbonate, water, brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationConcentration in vacuo 370 mg of 4-Ethyl-7-methyl-benzo[b]thiophen-5-ol, 98%

출처 및 근거

ORD 기록
ord-651e502f7b584262a7f0a27158831396
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524725B2

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