Sodium hydride → (6-Bromo-pyridazin-3-yloxy)-acetic acid tert-butyl ester

HRID 1931383노트

반응식

HRID 1931383 반응식
[C:1]([O:5][C:6](=[O:9])[CH2:7][OH:8])([CH3:4])([CH3:3])[CH3:2].[H-].[Na+].[Br:12][C:13]1[N:14]=[N:15][C:16](Br)=[CH:17][CH:18]=1>CN(C=O)C>[C:1]([O:5][C:6](=[O:9])[CH2:7][O:8][C:16]1[N:15]=[N:14][C:13]([Br:12])=[CH:18][CH:17]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 2488523,6-DibromopyridazineHCID 11815394Tert-butyl 2-hydroxyacetate

생성물 1

HCID 86638119(6-Bromo-pyridazin-3-yloxy)-acetic acid tert-butyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

277.8 mg (2.1 mmol) of hydroxyacetic acid tert-butyl ester and 100.9 mg of sodium hydride (55% in mineral oil) in 15 ml of DMF were stirred at room temperature for 30 min. Then 500 mg (2.1 mmol) of 3,6-dibromopyridazine were added, and the reaction mixture was stirred at 60° C. for 2 h. After evaporation to dryness, the residue was stirred with ethyl acetate, the solution filtered, evaporated, and the crude product (450 mg) directly employed in the subsequent step.

후처리

  1. customAfter evaporation to dryness
  2. stirringthe residue was stirred with ethyl acetate
  3. filtrationthe solution filtered
  4. customevaporated

출처 및 근거

ORD 기록
ord-caef1ec6fadf466eb1b44077cf0233c9
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188291B2

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