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

HRID 1677343

반응식

HRID 1677343 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 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 diethyl 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. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperatureto reflux for 30 min
  4. temperaturecooled
  5. washwashed with saturated sodium bicarbonate, water, brine
  6. dry with materialdried over magnesium sulfate
  7. concentrationConcentration in vacuo 370 mg of 4-Ethyl-7-methyl-benzo[b]thiophen-5-ol, 98%

출처 및 근거

ORD 기록
ord-eb2931835ea04874a5996b769a3dd1d1
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08008313B2

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