Hydrogen Peroxide → 4-[7-Ethyl-3-(4-methoxyphenyl)-2-methylpyrrolo[1,2-b]pyridazin-4-yl]benzamide

HRID 2250572노트

반응식

HRID 2250572 반응식
[CH2:1]([C:3]1[N:7]2[N:8]=[C:9]([CH3:28])[C:10]([C:20]3[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=3)=[C:11]([C:12]3[CH:19]=[CH:18][C:15]([C:16]#[N:17])=[CH:14][CH:13]=3)[C:6]2=[CH:5][CH:4]=1)[CH3:2].[OH-:29].[Na+].OO>CN(C)C=O>[CH2:1]([C:3]1[N:7]2[N:8]=[C:9]([CH3:28])[C:10]([C:20]3[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=3)=[C:11]([C:12]3[CH:19]=[CH:18][C:15]([C:16]([NH2:17])=[O:29])=[CH:14][CH:13]=3)[C:6]2=[CH:5][CH:4]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 688027564-[7-Ethyl-3-(4-methoxyphenyl)-2-methylpyrrolo[1,2-b]pyridazin-4-yl]benzonitrile

생성물 1

HCID 688035184-[7-Ethyl-3-(4-methoxyphenyl)-2-methylpyrrolo[1,2-b]pyridazin-4-yl]benzamide수율 78%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-[7-ethyl-3-(4-methoxyphenyl)-2-methylpyrrolo[1,2-b]pyridazin-4-yl]benzonitrile (22 mg) in N,N-dimethylformamide (1 mL) were added 1N sodium hydroxide (0.12 mL) and 30% hydrogen peroxide (0.07 mL) at ambient temperature. After 1 hour stirring, the reaction mixture was partitioned between ethyl acetate and water. The organic layer was washed with water three times and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by flash silica gel column chromatography (silica gel, 30 mL) eluting with hexane-ethyl acetate=5-1 and 0-1 to give 4-[7-ethyl-3-(4-methoxyphenyl)-2-methylpyrrolo[1,2-b]pyridazin-4-yl]benzamide (18 mg, 78.0%) as an yellow solid.

후처리

  1. customthe reaction mixture was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with water three times and brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was purified by flash silica gel column chromatography (silica gel, 30 mL)
  6. washeluting with hexane-ethyl acetate=5-1 and 0-1

출처 및 근거

ORD 기록
ord-7ee29a720dab4f6eabfc6dde43e8295a
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07317009B2

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