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

HRID 1931383ノート

反応式

HRID 1931383 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-caef1ec6fadf466eb1b44077cf0233c9
出典データセット
uspto-grants-2012_05
特許番号
US08188291B2

反応ノート

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