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Potassium Carbonate → (5-Chloro-6-ethyl-3-pyridinyl)methanol

HRID 420732
ノート
印刷プレビュー

反応式

HRID 420732 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][OH:10])[CH:5]=[N:6][C:7]=1Cl.C([O-])([O-])=O.[K+].[K+].[CH2:17]([Zn]CC)[CH3:18]>C1COCC1>[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][OH:10])[CH:5]=[N:6][C:7]=1[CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 21882961(5,6-Dichloropyridin-3-yl)methanolHCID 178418750HCID 178418750、化合物

生成物 1

HCID 59698822(5-Chloro-6-ethyl-3-pyridinyl)methanol収率 21.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of (5,6-dichloro-3-pyridinyl)methanol (500 mg, 2.81 mmol), K2CO3 (1165 mg, 8.43 mmol), and [1,1′-Bis(diphenylphosphino) ferrocene]dichloro-palladium(II) (206 mg, 0.281 mmol) in THF (17 ml), was added diethylzinc (5.67 ml, 5.67 mmol). The mixture was stirred under reflux for 16 h in a pressure tube. The resulting mixture was quenched upon the addition of aqueous HCl until pH 7 and extracted with EtOAc. The combined organic layers were washed with brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by flash chromatography using Flashmaster II, spherical silica gel cartridge BP-SUP 20-40μ, and mixtures of EtOAc and hexane as eluents to give 103 mg of desired compound.

後処理

  1. temperatureunder reflux for 16 h in a pressure tube
  2. customThe resulting mixture was quenched upon the addition of aqueous HCl until pH 7
  3. extractionextracted with EtOAc
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography

出典と根拠

ORDレコード
ord-c4da075870714262a2c6c1bd8bfc9dee
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08097628B2

反応ノート

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