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Potassium Carbonate → 6-(Hydroxymethyl)-3-methylpyridine-2-carbonitrile

HRID 2356633
ノート
印刷プレビュー

反応式

HRID 2356633 の反応式
C(=O)([O-])[O-].[K+].[K+].C([O:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([C:19]#[N:20])[N:13]=1)(=O)C>CO>[OH:10][CH2:11][C:12]1[N:13]=[C:14]([C:19]#[N:20])[C:15]([CH3:18])=[CH:16][CH:17]=1
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 11430Potassium CarbonateHCID 68457380(6-Cyano-5-methyl-2-pyridinyl)methyl acetate

生成物 1

HCID 573366546-(Hydroxymethyl)-3-methylpyridine-2-carbonitrile収率 80.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium carbonate (82 mg) was added to a solution of (6-cyano-5-methyl-2-pyridinyl)methyl acetate (3.62 g) in methanol (25 ml) and the mixture stirred under argon at ambient temperature for 2 hours. It was concentrated in vacuo to ca. ¼ volume and water (50 ml) added. The mixture was neutralized with 5% acetic acid (1.5 ml) and extracted with dichloromethane (50 ml then 2×25 ml). The combined extracts were washed with brine (25 ml), dried (MgSO4) and concentrated in vacuo. The residue was recrystallised from ether:hexane to afford the title compound (2.26 g, 80%) as a pale buff solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. concentrationIt was concentrated in vacuo to ca. ¼ volume and water (50 ml)
  2. additionadded
  3. extractionextracted with dichloromethane (50 ml
  4. washThe combined extracts were washed with brine (25 ml)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was recrystallised from ether

出典と根拠

ORDレコード
ord-7c9d407ef1f14dfd88a1061dbfac36d0
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07759369B2

反応ノート

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