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

HRID 81842

反応式

HRID 81842 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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%

出典と根拠

ORDレコード
ord-83efcba7df024aaea959acc41fb64be0
出典データセット
uspto-grants-2014_09
特許番号
US08846705B2

関連ノート

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