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

HRID 2176882노트

반응식

HRID 2176882 반응식
[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

참가 물질

3

반응물 2

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

생성물 1

HCID 673832592-(6-Methoxypyridin-3-yl)acetamide수율 52.2%

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-900f435d1ed544e8bb7bcccb90c0fc46
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09067888B2

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