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

HRID 1351076ノート

反応式

HRID 1351076 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 hydrazine hydrate (99%), dissolved in 1 ml of ethanol, is added dropwise at ambient temperature to a solution of 1.80 g of methyl 2-bromo-3-(2-butyn-1-yl)-5-formyl-3H-imidazol-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 solid precipitated 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 solid
  3. customprecipitated
  4. filtrationfiltered
  5. washwashed with 10 ml of ethanol and 20 ml of diethyl ether
  6. customdried

出典と根拠

ORDレコード
ord-4004c3d3462942e29953efc377697ac8
出典データセット
uspto-grants-2007_05
特許番号
US07217711B2

反応ノート

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