Acetic Acid → 2-Bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

HRID 350663ノート

反応式

HRID 350663 の反応式
O.[NH2:2][NH2:3].[Br:4][C:5]1[N:9]([CH2:10][C:11]#[C:12][CH3:13])[C:8]([C:14]([O:16]C)=O)=[C:7]([CH:18]=O)[N:6]=1.C(O)(=O)C>C(O)C>[Br:4][C:5]1[N:9]([CH2:10][C:11]#[C:12][CH3:13])[C:8]2[C:14](=[O:16])[NH:3][N:2]=[CH:18][C:7]=2[N:6]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 21947682methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylate

生成物 1

HCID 219476582-Bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

0.31 ml of hydrazine hydrate (99%), dissolved in 1 ml of ethanol, are added dropwise at ambient temperature to a solution of 1.80 g of methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazole-4-carboxylate in 25 ml of ethanol. Five minutes later 1.5 ml of concentrated acetic acid are added and the mixture is refluxed for 30 minutes. After cooling the precipitated solid is suction filtered, washed with 10 ml of ethanol and 20 ml of diethyl ether and dried.

後処理

  1. temperaturethe mixture is refluxed for 30 minutes
  2. temperatureAfter cooling the precipitated solid
  3. filtrationfiltered
  4. washwashed with 10 ml of ethanol and 20 ml of diethyl ether
  5. customdried

出典と根拠

ORDレコード
ord-69a4d8058cb64f0cb04c9d95639208a8
出典データセット
uspto-grants-2007_02
特許番号
US07183280B2

反応ノート

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