Sodium Iodide → HCID 20435938、化合物

HRID 1154037ノート

反応式

HRID 1154037 の反応式
CS(O[CH2:6][CH2:7][C:8]1([CH3:23])[C:20](=[O:21])[N:11]2[CH2:12][CH:13]=[CH:14][CH:15]([C:16]([O:18][CH3:19])=[O:17])[N:10]2[C:9]1=[O:22])(=O)=O.[I-:24].[Na+]>CC(C)=O>[I:24][CH2:6][CH2:7][C:8]1([CH3:23])[C:20](=[O:21])[N:11]2[CH2:12][CH:13]=[CH:14][CH:15]([C:16]([O:18][CH3:19])=[O:17])[N:10]2[C:9]1=[O:22]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 20435967HCID 20435967、化合物

生成物 1

HCID 20435938HCID 20435938、化合物収率 80.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 7.6 g (22 mmol) of methyl 2,3,5,8-tetrahydro-2-(2-methanesulfonyloxyethyl)-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate and 6.6 g (44 mmol) of sodium iodide in 100 ml of acetone was heated under reflux for 16 hours. The resulting suspension was filtered and the filtrate was evaporated to dryness. The residue was partitioned between dichloromethane and water. The organic solution was washed with 10% aqueous sodium thiosulfate, dried over magnesium sulfate and evaporated to give 6.7 g (80%) of methyl 2,3,5,8-tetrahydro-2-(2-iodoethyl)-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]-pyridazine-5-carboxylate having a melting point of 86°-87° C. (from diethyl ether).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hours
  3. filtrationThe resulting suspension was filtered
  4. customthe filtrate was evaporated to dryness
  5. customThe residue was partitioned between dichloromethane and water
  6. washThe organic solution was washed with 10% aqueous sodium thiosulfate
  7. dry with materialdried over magnesium sulfate
  8. customevaporated

出典と根拠

ORDレコード
ord-6bdb3861728946d3be8fad82ffb50c1f
出典データセット
uspto-grants-1984_12
特許番号
US04487929

反応ノート

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