Potassium Carbonate → HCID 68458843、化合物

HRID 2356627ノート

反応式

HRID 2356627 の反応式
C(=O)([O-])[O-].[K+].[K+].C([O:10][CH2:11][C:12]1[C:17]([CH3:18])=[CH:16][CH:15]=[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])[CH:15]=[CH:16][C:17]=1[CH3:18]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 68457478(6-Cyano-3-methyl-2-pyridinyl)methyl acetate

生成物 1

HCID 68458843HCID 68458843、化合物収率 64.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Potassium carbonate (65 mg) was added to a solution of (6-cyano-3-methyl-2-pyridinyl)methyl acetate (2.89 g) in methanol (20 ml) and the mixture stirred under argon at ambient temperature for 2.5 hours. It was concentrated in vacuo to ca. ½ volume and water (40 ml) added. The mixture was neutralized with 5% acetic acid (1.2 ml) and extracted with dichloromethane (40 ml then 2×20 ml). The combined extracts were washed with brine (20 ml), dried (MgSO4) and concentrated in vacuo. The residue was purified by Biotage chromatography eluting with 2:1 hexane:ethyl acetate to afford the title compound (1.45 g, 64%) as a pale buff solid. LC/MS [MH+]=149, RT=1.46 min.

後処理

  1. concentrationIt was concentrated in vacuo to ca. ½ volume and water (40 ml)
  2. additionadded
  3. extractionextracted with dichloromethane (40 ml
  4. washThe combined extracts were washed with brine (20 ml)
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by Biotage chromatography
  8. washeluting with 2:1 hexane

出典と根拠

ORDレコード
ord-9e0994d735094a519d98eaf2f04cce2b
出典データセット
uspto-grants-2010_07
特許番号
US07759369B2

反応ノート

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