Triethylamine → 2-Methylpyridine-4-carboxylic acid

HRID 273088

反応式

HRID 273088 の反応式
[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

参加物

6

反応物 3

HCID 8471TriethylamineHCID 1412092-Chloro-6-methylpyridine-4-carboxylic acidHCID 178418361HCID 178418361、化合物

生成物 1

HCID 27628212-Methylpyridine-4-carboxylic acid

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-3db16f75d17b4f68b39d141a45c58893
出典データセット
uspto-grants-2008_11
特許番号
US07456200B2

関連ノート

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