Hydrochloric Acid → 3-(2-Ethylpyrid-3-ylamino)-6-methyl-1-(carboxymethyl)pyrazinone

HRID 398389ノート

反応式

HRID 398389 の反応式
[CH2:1]([C:3]1[C:8]([NH:9][C:10]2[C:11](=[O:23])[N:12]([CH2:17][C:18]([O:20]CC)=[O:19])[C:13]([CH3:16])=[CH:14][N:15]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2].CO.[OH-].[Na+].Cl>O>[CH2:1]([C:3]1[C:8]([NH:9][C:10]2[C:11](=[O:23])[N:12]([CH2:17][C:18]([OH:20])=[O:19])[C:13]([CH3:16])=[CH:14][N:15]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 230001643-(2-Ethylpyrid-3-ylamino)-6-methyl-1-(ethoxycarbonylmethyl)pyrazinone

生成物 1

HCID 230002023-(2-Ethylpyrid-3-ylamino)-6-methyl-1-(carboxymethyl)pyrazinone収率 73.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 3-(2-Ethylpyrid-3-ylamino)-6-methyl-1-(ethoxycarbonylmethyl)pyrazinone (0.058 g, 0.183 mMol) from step 3 above in 6 mL of 1:1:1-tetrahydrofuran:methanol:water was added 183 μL (0.183 mMol) of 1N sodium hydroxide solution. The solution was stirred at ambient temperature for 18 h at which time 183 μL (0.183 mMol) of 1N hydrochloric acid solution was added. The solution was concentrated in vacuo several times from methanol and the residue was triturated with diethyl ether. The resulting precipitate was filtered off to afford the title compound as a beige powder (0.039 g; HPLC RT=3.13 min, method A).

後処理

  1. additionwas added
  2. concentrationThe solution was concentrated in vacuo several times from methanol
  3. customthe residue was triturated with diethyl ether
  4. filtrationThe resulting precipitate was filtered off

出典と根拠

ORDレコード
ord-b8f4923dc0dc4367bf2a218e6c688d81
出典データセット
uspto-grants-2003_08
特許番号
US06610692B1

反応ノート

読み込み中…