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

HRID 2356633
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HRID 2356633 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 68457380(6-Cyano-5-methyl-2-pyridinyl)methyl acetate

생성물 1

HCID 573366546-(Hydroxymethyl)-3-methylpyridine-2-carbonitrile수율 80.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-7c9d407ef1f14dfd88a1061dbfac36d0
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759369B2

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