Hydrochloric Acid → (E)-3-(6-Amino4-methylpyridin-3-yl)acrylic acid HCl salt

HRID 1761088

反応式

HRID 1761088 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([O:12]CC)=[O:11])=[C:4]([CH3:15])[CH:3]=1.[ClH:16]>CC(O)=O>[ClH:16].[NH2:1][C:2]1[N:7]=[CH:6][C:5](/[CH:8]=[CH:9]/[C:10]([OH:12])=[O:11])=[C:4]([CH3:15])[CH:3]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 57440845Ethyl (E)-3-(6-amino-4-methylpyridin-3-yl)acrylate

生成物 1

HCID 67343018(E)-3-(6-Amino4-methylpyridin-3-yl)acrylic acid HCl salt

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °C

実験手順

To ethyl (E)-3-(6-amino-4-methylpyridin-3-yl)acrylate (1.50 g, 7.3 mmole) was added HOAc (15 mL) and conc. HCl (15 mL). The solution was stirred at 100° C. for 10 hr, cooled to RT, and concentrated to dryness. Trituration with Et2O, filtration and drying under vacuum gave the title compound (1.65 g, quantitative) as a white solid: LCMS (ES) m/e 179.2 (M+H)+; 1H NMR (400 MHz, DMSO-d6) δ 8.37 (s,1H), 8.28 (br s, 3H), 7.51 (d, I=16.0 Hz,1H), 6.86 (s,1H), 6.46 (d, J=16.0 Hz,1H), 2.41 (s, 3H).

後処理

  1. temperaturecooled to RT
  2. concentrationconcentrated to dryness
  3. filtrationTrituration with Et2O, filtration
  4. customdrying under vacuum

出典と根拠

ORDレコード
ord-024ee6a331b844788d9b8b7999b46d69
出典データセット
uspto-grants-2005_01
特許番号
US06846819B1

関連ノート

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