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

HRID 12269

反応式

HRID 12269 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8366a1b2fef4b479476f79a57cde650
出典データセット
uspto-grants-2010_06
特許番号
US07727989B2

関連ノート

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