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

HRID 398389노트

반응식

HRID 398389 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-b8f4923dc0dc4367bf2a218e6c688d81
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610692B1

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