Sodium Bicarbonate → 2-(6-Methoxypyridin-3-yl)acetamide

HRID 2176882ノート

反応式

HRID 2176882 の反応式
[CH3:1][O:2][C:3]1[N:8]=[CH:7][C:6]([CH2:9][C:10]#[N:11])=[CH:5][CH:4]=1.C(=O)(O)[O-:13].[Na+]>>[CH3:1][O:2][C:3]1[N:8]=[CH:7][C:6]([CH2:9][C:10]([NH2:11])=[O:13])=[CH:5][CH:4]=1

参加物

3

反応物 2

HCID 516892Sodium BicarbonateHCID 45079846(6-Methoxypyridin-3-yl)acetonitrile

生成物 1

HCID 673832592-(6-Methoxypyridin-3-yl)acetamide収率 52.2%

実験手順

The compound 2-(6-methoxypyridin-3-yl)acetonitrile (0.60 g, 4.05 mmol) in poly phosphoric acid (6 g) was stirred at 95° C. for 1 h. The reaction mixture was neutralized with saturated sodium bicarbonate solution and the compound was extracted with DCM (3×20 ml). The combined organic layers were washed with brine (15 ml), dried over anhydrous sodium sulfate, filtered and concentrated under vacuo. The crude compound was washed with ether (2×5 ml) to afford 350 mg (52.2%) of 2-(6-methoxypyridin-3-yl)acetamide as white color solid.

後処理

  1. extractionthe compound was extracted with DCM (3×20 ml)
  2. washThe combined organic layers were washed with brine (15 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuo
  6. washThe crude compound was washed with ether (2×5 ml)

出典と根拠

ORDレコード
ord-900f435d1ed544e8bb7bcccb90c0fc46
出典データセット
uspto-grants-2015_06
特許番号
US09067888B2

反応ノート

読み込み中…