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

HRID 1677343

反応式

HRID 1677343 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 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.

後処理

  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%

出典と根拠

ORDレコード
ord-eb2931835ea04874a5996b769a3dd1d1
出典データセット
uspto-grants-2011_08
特許番号
US08008313B2

関連ノート

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