1-Trityl-4-ethoxymethylpyrazole → 4-Ethoxymethylpyrazole

HRID 570075

反応式

HRID 570075 の反応式
C([N:20]1[CH:24]=[C:23]([CH2:25][O:26][CH2:27][CH3:28])[CH:22]=[N:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>C(O)C.CC(C)=O.Cl>[CH2:27]([O:26][CH2:25][C:23]1[CH:24]=[N:20][NH:21][CH:22]=1)[CH3:28]

参加物

4

反応物 1

HCID 685285131-Trityl-4-ethoxymethylpyrazole

生成物 1

HCID 685328294-Ethoxymethylpyrazole収率 44%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 21889777Acetone ethanol溶媒

反応条件

温度
80 °C

実験手順

1-trityl-4-ethoxymethylpyrazole (1.800 g, 4.88 mmol) was dissolved in a mixture of ethanol/acetone (15 ml/5 ml) and 30 mL of 2N HCl was added to the resulting solution. The mixture was heated at 80° C. for 2 h. After cooling to room temperature, the reaction mixture was filtered and washed with dichloromethane. The aqueous layer was basified with 2N NaOH and extracted with dichloromethane. The organic layers were combined, dried over MgSO4 and the solvent was evaporated under vacuum yielding compound 4-ethoxymethylpyrazole as a white oil. Yield: 44% (270 mg, 2.14 mmol).

後処理

  1. additionwas added to the resulting solution
  2. temperatureAfter cooling to room temperature
  3. filtrationthe reaction mixture was filtered
  4. washwashed with dichloromethane
  5. extractionextracted with dichloromethane
  6. dry with materialdried over MgSO4
  7. customthe solvent was evaporated under vacuum

出典と根拠

ORDレコード
ord-852f47be86574ff68e08c58c5bd293f0
出典データセット
uspto-grants-2015_05
特許番号
US09023315B2

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