Sodium Hydroxide → HCID 58425466、化合物

HRID 1191174

反応式

HRID 1191174 の反応式
C([O:3][C:4]([C:6]1[N:7]([CH3:16])[N:8]=[C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])[C:10]=1[F:11])=[O:5])C.[OH-].[Na+]>CO>[C:12]([C:9]1[C:10]([F:11])=[C:6]([C:4]([OH:5])=[O:3])[N:7]([CH3:16])[N:8]=1)([CH3:15])([CH3:13])[CH3:14]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 674133345-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester

生成物 1

HCID 58425466HCID 58425466、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid ethyl ester (61.4 mg, 0.269 mmol, prepared as described in the previous step) was dissolved in MeOH (1 mL) then 2 M NaOH (175 μL, 0.350 mmol) was added. The resulting mixture was stirred at room temperature for 18 h and the solvent was removed under reduced pressure. The resulting residue was dissolved in H2O (10 mL) and acidified to pH ˜2 using 3 M HCl. The aqueous layer was extracted with DCM (3×5 mL), the combined organic extracts were dried over MgSO4 and filtered. The solvent was removed under reduced pressure to yield 5-tert-Butyl-4-fluoro-2-methyl-2H-pyrazole-3-carboxylic acid. 1H-NMRH-NMR (400 MHz, CDCl3) δ: 9.89 (br. s., 1H), 4.06 (d, J=1.0 Hz, 3H), 1.36 (s, 9H).

後処理

  1. customthe solvent was removed under reduced pressure
  2. dissolutionThe resulting residue was dissolved in H2O (10 mL)
  3. extractionThe aqueous layer was extracted with DCM (3×5 mL)
  4. dry with materialthe combined organic extracts were dried over MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-2fffa7d260cb4d908bc28be02cd17586
出典データセット
uspto-grants-2014_03
特許番号
US08680098B2

関連ノート

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