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Triethylamine → 2-Methylpyridine-4-carboxylic acid

HRID 273088
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HRID 273088 반응식
[H][H].Cl[C:4]1[CH:9]=[C:8]([C:10]([OH:12])=[O:11])[CH:7]=[C:6]([CH3:13])[N:5]=1.C(N(CC)CC)C>[Pd].C(O)C>[CH3:13][C:6]1[N:5]=[CH:4][CH:9]=[C:8]([C:10]([OH:12])=[O:11])[CH:7]=1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 1412092-Chloro-6-methylpyridine-4-carboxylic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 27628212-Methylpyridine-4-carboxylic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A hydrogen filled balloon was attached to a flask containing 2-chloro-6-methylpyridine-4-carboxylic acid (2 g, 12.0 mmol), palladium 10 wt. % on activated carbon (0.5 g), triethyl amine (4.8 ml) and ethanol (24 ml) and then stirred overnight at room temperature. The is reaction mixture was filtered through celite, washed with methanol and concentrated. The residue was titurated with dichloromethane and then filtered to afford 6-methylpyridine-4-carboxylic acid as a white solid; 1.05 g (66%). 1H NMR (MeOD) δ (ppm): 8.62 (d, 1H), 7.68 (s, 1H), 7.60 (d, 1H), 2.55 (s, 3H).

후처리

  1. customThe is reaction mixture
  2. filtrationwas filtered through celite
  3. washwashed with methanol
  4. concentrationconcentrated
  5. filtrationfiltered

출처 및 근거

ORD 기록
ord-3db16f75d17b4f68b39d141a45c58893
출처 데이터셋
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07456200B2

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