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Sodium Methoxide → 1-tert-butyl-5-methoxymethyl-1H-pyrazole-4-carboxylic acid

HRID 12872
ノート
印刷プレビュー

反応式

HRID 12872 の反応式
C[O:2][C:3]([C:5]1[CH:6]=[N:7][N:8]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:9]=1[CH2:10]Br)=[O:4].[CH3:16][O-:17].[Na+]>>[C:12]([N:8]1[C:9]([CH2:10][O:17][CH3:16])=[C:5]([C:3]([OH:2])=[O:4])[CH:6]=[N:7]1)([CH3:15])([CH3:14])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 10942334Sodium MethoxideHCID 670210095-bromomethyl-1-tert-butyl-1H-pyrazole-4-carboxylic acid methyl ester

生成物 1

HCID 670208941-tert-butyl-5-methoxymethyl-1H-pyrazole-4-carboxylic acid収率 88.6%

実験手順

A solution of 5-bromomethyl-1-tert-butyl-1H-pyrazole-4-carboxylic acid methyl ester (1.51 g, 5.48 mmol) (as prepared in Example 55, Step 1) in sodium methoxide (23.8 mL, 11.9 mmol, 0.5M solution in methanol) was warmed to 90° C. where it was stirred for 2.5 h. At this time, the reaction was concentrated in vacuo. The resulting white solids were taken up in water (100 mL) and extracted with ethyl acetate (1×150 mL). The organics were then washed with a saturated aqueous sodium bicarbonate solution (1×100 mL), water (1×100 mL) and a saturated aqueous sodium chloride solution (1×100 mL), dried over magnesium sulfate, filtered and concentrated in vacuo. When it was discovered that the product was not in the organic extracts, the aqueous layers were combined and were acidified to pH=1 with concentrated aqueous hydrochloric acid and then were extracted with dichloromethane (1×150 mL). These organics were dried over magnesium sulfate, filtered and concentrated in vacuo to afford 1-tert-butyl-5-methoxymethyl-1H-pyrazole-4-carboxylic acid (1.03 g, 88%) as a white solid. The material was used without further purification.

後処理

  1. concentrationAt this time, the reaction was concentrated in vacuo
  2. extractionextracted with ethyl acetate (1×150 mL)
  3. washThe organics were then washed with a saturated aqueous sodium bicarbonate solution (1×100 mL), water (1×100 mL)
  4. dry with materiala saturated aqueous sodium chloride solution (1×100 mL), dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. extractionwere extracted with dichloromethane (1×150 mL)
  8. dry with materialThese organics were dried over magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-baceeafd53ab43f0bc5472498653cd1c
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07728029B2

反応ノート

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