홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Methyl iodide → Ethyl 1-methyl-6-oxo-1,6-dihydropyridazine-4-carboxylate

HRID 2243893
노트
인쇄 미리보기

반응식

HRID 2243893 반응식
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][NH:9][C:10](=[O:12])[CH:11]=1)=[O:5])[CH3:2].[C:13](=O)([O-])[O-].[K+].[K+].CI.C(OCC)(=O)C>CN(C=O)C.O>[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH3:13])[C:10](=[O:12])[CH:11]=1)=[O:5])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 12376258Ethyl 6-oxo-1,6-dihydropyridazine-4-carboxylate

생성물 1

HCID 59006703Ethyl 1-methyl-6-oxo-1,6-dihydropyridazine-4-carboxylate수율 66.2%

시약·촉매·용매 2

HCID 962Water
용매
HCID 6228Dimethylformamide용매

반응 조건

온도
0 °C

실험 절차

To a stirred solution of 6-oxo-1,6-dihydro-pyridazine-4-carboxylic acid ethyl ester (1.0 g, 5.9 mmol) in anhydrous DMF (15 mL) was added potassium carbonate (3.29 g, 23.8 mmol). The reaction mixture was cooled to 0° C. and methyl iodide (1.0 mL, 16 mmol) was added dropwise. The reaction mixture was allowed to reach room temperature and was then heated at 60° C. for 15 minutes. The reaction was cooled to below 0° C. and ethyl acetate and water were added. The organic layer was separated, washed with cold water and brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified by RP-HPLC using a linear gradient of acetonitrile in 0.1 M ammonium acetate buffer to afford the title compound (712 mg, 66%).

후처리

  1. customto reach room temperature
  2. temperaturewas then heated at 60° C. for 15 minutes
  3. temperatureThe reaction was cooled to below 0° C.
  4. customThe organic layer was separated
  5. washwashed with cold water and brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. concentrationconcentrated
  8. customThe residue was purified by RP-HPLC

출처 및 근거

ORD 기록
ord-11b4e6a2b91744eba563880f49a24a0f
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07678796B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트