Hydrochloric Acid → 3-Ethynylbenzonitrile

HRID 606787

反応式

HRID 606787 の反応式
C(=O)([O-])[O-].[K+].[K+].C[Si]([C:11]#[C:12][C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])(C)C.Cl>CO>[C:12]([C:13]1[CH:14]=[C:15]([CH:18]=[CH:19][CH:20]=1)[C:16]#[N:17])#[CH:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 225703183-[(Trimethylsilyl)ethynyl]benzonitrile

生成物 1

HCID 120889643-Ethynylbenzonitrile収率 92%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Add potassium carbonate (0.138 g, 1 mmol) to a solution of 3-trimethylsilanylethynylbenzonitrile from PREPARATION 5 (2.0 g, 10.1 mmol) in methanol (50 mL). Stir the mixture at room temperature for 20 min and add a 10% aqueous hydrochloric acid solution (4 mL). Concentrate to a reduced volume, add diethyl ether and water and separate the phases. Wash once the aqueous phase with diethyl ether. Combine the organic phases, dry over sodium sulfate and concentrate to obtain the title compound as a solid (1.17 g, 92%).

後処理

  1. concentrationConcentrate to a reduced volume
  2. additionadd diethyl ether and water
  3. customseparate the phases
  4. washWash once the aqueous phase with diethyl ether
  5. dry with materialdry over sodium sulfate
  6. concentrationconcentrate

出典と根拠

ORDレコード
ord-0eabd544b1254993971a164e6b861429
出典データセット
uspto-grants-2011_03
特許番号
US07915424B2

関連ノート

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