Potassium Carbonate → HCID 68458843, 화합물

HRID 2356627노트

반응식

HRID 2356627 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 68458843HCID 68458843, 화합물수율 64.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9e0994d735094a519d98eaf2f04cce2b
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759369B2

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