HCID 20435938, 화합물 → HCID 20435958, 화합물

HRID 1154038노트

반응식

HRID 1154038 반응식
I[CH2:2][CH2:3][C:4]1([CH3:19])[C:16](=[O:17])[N:7]2[CH2:8][CH:9]=[CH:10][CH:11]([C:12]([O:14][CH3:15])=[O:13])[N:6]2[C:5]1=[O:18].[C:20]([O-:23])(=[S:22])[CH3:21].[K+]>CC(C)=O>[C:20]([S:22][CH2:2][CH2:3][C:4]1([CH3:19])[C:16](=[O:17])[N:7]2[CH2:8][CH:9]=[CH:10][CH:11]([C:12]([O:14][CH3:15])=[O:13])[N:6]2[C:5]1=[O:18])(=[O:23])[CH3:21]

참가 물질

4

반응물 2

HCID 20435938HCID 20435938, 화합물HCID 23670855Potassium ethanethioate

생성물 1

HCID 20435958HCID 20435958, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 6.43 g (17 mmol) of methyl 2,3,5,8-tetrahydro-2-(2-iodoethyl)-2-methyl-1,3-dioxo-1H-pyrazolo-[1,2-a]pyridazine-5-carboxylate and 1.94 g (17 mmol) of potassium thioacetate in 150 ml of acetone was stirred at room temperature for 5 hours. The solvent was removed by evaporation and the residue was partitioned between dichloromethane and water. The organic phase was separated, dried over magnesium sulfate and evaporated to give methyl 2-(2-acetylthioethyl)-2,3,5,8-tetrahydro-2-methyl-1,3-dioxo-1H-pyrazolo[1,2-a]pyridazine-5-carboxylate as a mixture of diastereomers. Chromatography on silica gel using diethyl ether for the elution gave 3.81 g (69%) of diastereomer A in the form of a colorless oil and 1.26 g (23%) of diastereomer B in the form of a colorless oil.

후처리

  1. customThe solvent was removed by evaporation
  2. customthe residue was partitioned between dichloromethane and water
  3. customThe organic phase was separated
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-83365bed99c5426eb7831fa2567c86a2
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04487929

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