Sodium Iodide → HCID 20435938, 화합물

HRID 1154037노트

반응식

HRID 1154037 반응식
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]

참가 물질

4

반응물 2

HCID 5238Sodium IodideHCID 20435967HCID 20435967, 화합물

생성물 1

HCID 20435938HCID 20435938, 화합물수율 80.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6bdb3861728946d3be8fad82ffb50c1f
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487929

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