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2-(1-Methylindol-2-yl)propan-2-ol → HCID 10464759、化合物

HRID 373996
ノート
印刷プレビュー

反応式

HRID 373996 の反応式
O[C:2]([C:5]1[N:6]([CH3:14])[C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)([CH3:4])[CH3:3].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[C:2]([C:5]1[N:6]([CH3:14])[C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)([CH3:4])=[CH2:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2956452-(1-Methylindol-2-yl)propan-2-olHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 10464759HCID 10464759、化合物収率 24%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4.0 g of 2-(1-hydroxy-1-methylethyl)-1-methylindole was dissolved in 80 ml of toluene. Thereto was added 200 mg of p-toluenesulfonic acid monohydrate. The mixture was azeotropically refluxed for 2 hours. The reaction mixture was cooled to room temperature, washed with an aqueous saturated sodium hydrogencarbonate solution and an aqueous saturated sodium chloride solution in this order, and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure. The residue was purified by column chromatography (eluant: n-hexane/toluene=1/0 to 20/1) to obtain 850 mg (yield: 24%) of 2-isopropenyl-1-methylindole as a light yellow oily material.

後処理

  1. temperatureThe mixture was azeotropically refluxed for 2 hours
  2. washwashed with an aqueous saturated sodium hydrogencarbonate solution
  3. dry with materialan aqueous saturated sodium chloride solution in this order, and dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. customThe residue was purified by column chromatography (eluant: n-hexane/toluene=1/0 to 20/1)

出典と根拠

ORDレコード
ord-5a48357e72464a30a0a416744e65ab50
出典データセット
uspto-grants-1992_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05166204

反応ノート

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