Sodium Hydroxide → 2,3-Dimethyl-8-(2-ethyl-6-methylbenzylamino)-imidazo[1,2-a]pyridine-6-carboxylic acid

HRID 427479

反応式

HRID 427479 の反応式
S(O)(=O)(=O)C.[CH2:6]([C:8]1[CH:29]=[CH:28][CH:27]=[C:26]([CH3:30])[C:9]=1[CH2:10][NH:11][C:12]1[C:13]2[N:14]([C:21]([CH3:25])=[C:22]([CH3:24])[N:23]=2)[CH:15]=[C:16]([C:18](N)=[O:19])[CH:17]=1)[CH3:7].[OH-:31].[Na+]>C(O)C>[CH2:6]([C:8]1[CH:29]=[CH:28][CH:27]=[C:26]([CH3:30])[C:9]=1[CH2:10][NH:11][C:12]1[C:13]2[N:14]([C:21]([CH3:25])=[C:22]([CH3:24])[N:23]=2)[CH:15]=[C:16]([C:18]([OH:19])=[O:31])[CH:17]=1)[CH3:7]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 99106658-(2-Ethyl-6-methylbenzylamino)-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxamide mesylate

生成物 1

HCID 118239362,3-Dimethyl-8-(2-ethyl-6-methylbenzylamino)-imidazo[1,2-a]pyridine-6-carboxylic acid収率 90.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

8-(2-ethyl-6-methylbenzylamino)-2,3-dimethylimidazo[1,2-a]pyridine-6-carboxamide mesylate (11.0 g, 0.025 mol) and sodium hydroxide (7.0 g, 0.17 mol) were solved in ethanol(95%) (120 ml) and was refluxed for 20 h. The solvent was evaporated under reduced pressure and to the residue was added water (150 ml). The pH was adjusted to 5 by addition of conc HCl and acetic acid and the solid that precipitated was isolated by filtration, washed with water and acetone, and dried to give 7.6 g (88%) of the title compound.

後処理

  1. temperaturewas refluxed for 20 h
  2. customThe solvent was evaporated under reduced pressure and to the residue
  3. additionwas added water (150 ml)
  4. additionThe pH was adjusted to 5 by addition of conc HCl and acetic acid
  5. customthe solid that precipitated
  6. customwas isolated by filtration
  7. washwashed with water and acetone
  8. customdried

出典と根拠

ORDレコード
ord-97ca8a2e41ff47da86c1f8d1414d5bed
出典データセット
uspto-grants-2001_11
特許番号
US06313136B1

関連ノート

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