Hydrazinium chloride → Ethyl 6-(2-ethylaminopyrimidin-4-yl)-3-oxo-2,3-dihydropyridazine-4-carboxylate

HRID 12269

반응식

HRID 12269 반응식
[CH2:1]([NH:3][C:4]1[N:9]=[C:8]([C:10](=O)[CH2:11][C:12](O)([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:13](OCC)=[O:14])[CH:7]=[CH:6][N:5]=1)[CH3:2].Cl.[NH2:26][NH2:27]>C(O)C>[CH2:1]([NH:3][C:4]1[N:9]=[C:8]([C:10]2[CH:11]=[C:12]([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:13](=[O:14])[NH:26][N:27]=2)[CH:7]=[CH:6][N:5]=1)[CH3:2]

참가 물질

4

반응물 2

HCID 115031Hydrazinium chlorideHCID 68452836Diethyl 2-[2-(2-ethylaminopyrimidin-4-yl)-2-oxo-ethyl]-2-hydroxymalonate

생성물 1

HCID 68453190Ethyl 6-(2-ethylaminopyrimidin-4-yl)-3-oxo-2,3-dihydropyridazine-4-carboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
130 °C

실험 절차

A mixture of 2 g of diethyl 2-[2-(2-ethylaminopyrimidin-4-yl)-2-oxo-ethyl]-2-hydroxy-malonate, 485 mg of hydrazine hydrochloride and 20 ml of ethanol is stirred under reflux for 24 hours. After cooling while stirring, the precipitate is filtered off with suction, heated in 4 ml of N-methylpyrrolidinone (NMP) at 130° C. for 3 hours and, after cooling, mixed with 15 ml of n-heptane and stirred. The precipitate is then filtered off with suction and stirred with methylene chloride, again filtered off with suction and dried.

후처리

  1. temperatureunder reflux for 24 hours
  2. temperatureAfter cooling
  3. stirringwhile stirring
  4. filtrationthe precipitate is filtered off with suction
  5. temperatureafter cooling
  6. additionmixed with 15 ml of n-heptane
  7. stirringstirred
  8. filtrationThe precipitate is then filtered off with suction
  9. stirringstirred with methylene chloride
  10. filtrationagain filtered off with suction
  11. customdried

출처 및 근거

ORD 기록
ord-d8366a1b2fef4b479476f79a57cde650
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07727989B2

연결된 노트

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